#------------------------------------------------------------------------------
#$Date: 2020-04-05 12:50:45 +0200 (dom 05 de abr de 2020) $
#$Revision: 250293 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/35/7703571.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_7703571
loop_
_publ_author_name
'Liu, Chao'
'Yang, Xin-Xue'
'Niu, Shuai'
'Yi, Xiao-Yi'
'Pan, Qing-Jiang'
_publ_section_title
;
 Occurrence of polyoxouranium motifs in uranyl organic networks
 constructed by using silicon-centered carboxylate linkers: structures,
 spectroscopy and computation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4155
_journal_page_last               4163
_journal_paper_doi               10.1039/d0dt00379d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C32 H12 O34 Si U6, 20(H2 O)'
_chemical_formula_sum            'C32 H52 O54 Si U6'
_chemical_formula_weight         2757.00
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc237nhj
_audit_creation_date             2020-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-19 deposited with the CCDC.	2020-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.9739(6)
_cell_length_b                   21.9739(6)
_cell_length_c                   37.455(2)
_cell_measurement_reflns_used    5996
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.62
_cell_volume                     18085.2(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            48805
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.854
_exptl_absorpt_coefficient_mu    10.805
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1487 before and 0.0632 after correction. The Ratio of minimum to maximum transmission is 0.5965. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9936
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.414
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0408P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3238
_reflns_number_total             3971
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt00379d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7703568--7703571.cif.'
_cod_original_cell_volume        18085.3(14)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               7703571
_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_max   0.140
_shelx_estimated_absorpt_t_min   0.075
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'
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
U1 U 0.66696(2) 0.43247(2) 0.47502(2) 0.02140(9) Uani 1 1 d . . . . .
U2 U 0.72897(2) 0.47897(2) 0.375000 0.02065(10) Uani 1 2 d S T P . .
Si1 Si 0.500000 0.750000 0.375000 0.0084(6) Uani 1 4 d S T P . .
O2 O 0.6721(2) 0.4221(2) 0.375000 0.0317(17) Uani 1 2 d S T P . .
O3 O 0.6541(2) 0.55234(19) 0.38982(12) 0.0278(11) Uani 1 1 d . . . . .
O3AA O 0.7860(2) 0.5360(2) 0.375000 0.0275(15) Uani 1 2 d S T P . .
O4 O 0.7121(2) 0.4937(2) 0.31578(12) 0.0269(10) Uani 1 1 d . . . . .
O5 O 0.6490(2) 0.36903(19) 0.44862(13) 0.0292(11) Uani 1 1 d . . . . .
O6 O 0.6837(2) 0.4951(2) 0.50304(12) 0.0289(11) Uani 1 1 d . . . . .
O7 O 0.6196(2) 0.4996(2) 0.43603(12) 0.0298(11) Uani 1 1 d . . . . .
O8 O 0.750000 0.3838(3) 0.500000 0.0213(14) Uani 1 2 d S T P . .
O9 O 0.37407(19) 0.6226(2) 0.47390(13) 0.0356(13) Uani 1 1 d . . . . .
O10 O 0.4368(2) 0.5628(2) 0.50244(13) 0.0333(12) Uani 1 1 d . . . . .
C1 C 0.4257(3) 0.5989(3) 0.47730(19) 0.0301(16) Uani 1 1 d . . . . .
C2 C 0.4749(3) 0.6141(3) 0.45058(17) 0.0220(14) Uani 1 1 d . . . . .
C3 C 0.4688(3) 0.6662(3) 0.42921(16) 0.0196(14) Uani 1 1 d . . . . .
H3 H 0.434482 0.691951 0.432260 0.024 Uiso 1 1 calc R . . . .
C4 C 0.5123(3) 0.6807(3) 0.40361(15) 0.0143(12) Uani 1 1 d . . . . .
C5 C 0.6159(3) 0.5438(3) 0.41502(16) 0.0204(14) Uani 1 1 d . . . . .
C6 C 0.5227(3) 0.5754(3) 0.44587(17) 0.0194(14) Uani 1 1 d . . . . .
H6 H 0.526729 0.540178 0.460402 0.023 Uiso 1 1 calc R . . . .
C7 C 0.5648(3) 0.5878(3) 0.42002(16) 0.0171(13) Uani 1 1 d . . . . .
C8 C 0.5610(2) 0.6401(2) 0.39923(16) 0.0142(12) Uani 1 1 d . . . . .
H8 H 0.591543 0.648401 0.381965 0.017 Uiso 1 1 calc R . . . .
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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
O4 U1 O9 155.08(15) 7_545 17_666 ?
O4 U1 O10 151.62(15) 7_545 17_666 ?
O5 U1 O4 90.87(18) . 7_545 ?
O5 U1 O6 177.8(2) . . ?
O5 U1 O7 92.82(19) . . ?
O5 U1 O8 92.18(18) . . ?
O5 U1 O9 87.97(19) . 17_666 ?
O5 U1 O10 91.07(19) . 17_666 ?
O6 U1 O4 91.18(18) . 7_545 ?
O6 U1 O7 88.43(19) . . ?
O6 U1 O8 87.45(18) . . ?
O6 U1 O9 89.86(19) . 17_666 ?
O6 U1 O10 87.47(18) . 17_666 ?
O7 U1 O4 74.87(15) . 7_545 ?
O7 U1 O9 130.04(14) . 17_666 ?
O7 U1 O10 76.75(15) . 17_666 ?
O8 U1 O4 79.99(12) . 7_545 ?
O8 U1 O7 154.42(13) . . ?
O8 U1 O9 75.19(11) . 17_666 ?
O8 U1 O10 128.22(11) . 17_666 ?
O10 U1 O9 53.30(14) 17_666 17_666 ?
O2 U2 O3 89.44(11) . . ?
O2 U2 O3 89.43(11) . 7_545 ?
O2 U2 O3AA 180.0 . . ?
O2 U2 O4 89.17(11) . . ?
O2 U2 O4 89.17(11) . 7_545 ?
O3 U2 O3 178.9(2) 7_545 . ?
O3AA U2 O3 90.56(11) . . ?
O3AA U2 O3 90.57(11) . 7_545 ?
O3AA U2 O4 90.83(11) . 7_545 ?
O3AA U2 O4 90.83(11) . . ?
O4 U2 O3 91.02(16) 7_545 7_545 ?
O4 U2 O3 91.03(16) . . ?
O4 U2 O3 88.96(16) 7_545 . ?
O4 U2 O3 88.96(16) . 7_545 ?
O4 U2 O4 178.3(2) 7_545 . ?
C4 Si1 C4 110.6(3) 10_564 . ?
C4 Si1 C4 108.91(17) 19_576 . ?
C4 Si1 C4 108.91(17) 19_576 10_564 ?
C4 Si1 C4 108.91(17) 28_656 . ?
C4 Si1 C4 108.91(17) 10_564 28_656 ?
C4 Si1 C4 110.6(3) 19_576 28_656 ?
C5 O3 U2 122.0(4) . . ?
U2 O4 U1 124.97(19) . 7_545 ?
C5 O7 U1 156.4(4) . . ?
U1 O8 U1 124.9(2) 5_656 . ?
C1 O9 U1 92.8(4) . 17_666 ?
C1 O10 U1 92.9(4) . 17_666 ?
O9 C1 U1 60.6(3) . 17_666 ?
O9 C1 O10 120.9(6) . . ?
O9 C1 C2 119.2(6) . . ?
O10 C1 U1 60.4(3) . 17_666 ?
O10 C1 C2 119.9(6) . . ?
C2 C1 U1 177.9(5) . 17_666 ?
C3 C2 C1 119.4(5) . . ?
C6 C2 C1 119.9(6) . . ?
C6 C2 C3 120.6(5) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(5) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 Si1 118.6(4) . . ?
C3 C4 C8 117.4(5) . . ?
C8 C4 Si1 123.9(4) . . ?
O3 C5 C7 119.4(5) . . ?
O7 C5 O3 122.4(5) . . ?
O7 C5 C7 118.1(5) . . ?
C2 C6 H6 120.4 . . ?
C2 C6 C7 119.3(5) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 C5 118.0(5) . . ?
C6 C7 C8 121.3(5) . . ?
C8 C7 C5 120.7(5) . . ?
C4 C8 H8 119.8 . . ?
C7 C8 C4 120.4(5) . . ?
C7 C8 H8 119.8 . . ?
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
U1 O4 2.368(4) 7_545 ?
U1 O5 1.754(5) . ?
U1 O6 1.769(5) . ?
U1 O7 2.322(4) . ?
U1 O8 2.313(3) . ?
U1 O9 2.437(4) 17_666 ?
U1 O10 2.434(4) 17_666 ?
U2 O2 1.766(6) . ?
U2 O3 2.369(4) . ?
U2 O3 2.369(4) 7_545 ?
U2 O3AA 1.774(6) . ?
U2 O4 2.272(4) . ?
U2 O4 2.272(4) 7_545 ?
Si1 C4 1.882(6) . ?
Si1 C4 1.882(6) 10_564 ?
Si1 C4 1.882(6) 19_576 ?
Si1 C4 1.882(6) 28_656 ?
O3 C5 1.277(7) . ?
O7 C5 1.253(7) . ?
O9 C1 1.255(8) . ?
O10 C1 1.256(8) . ?
C1 C2 1.510(8) . ?
C2 C3 1.402(8) . ?
C2 C6 1.365(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.391(8) . ?
C4 C8 1.402(7) . ?
C5 C7 1.493(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.366(8) . ?
C7 C8 1.391(8) . ?
C8 H8 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O7 C5 O3 47.7(14) . . . . ?
U1 O7 C5 C7 -132.2(9) . . . . ?
U1 O9 C1 O10 -2.1(7) 17_666 . . . ?
U1 O9 C1 C2 177.6(6) 17_666 . . . ?
U1 O10 C1 O9 2.1(7) 17_666 . . . ?
U1 O10 C1 C2 -177.6(6) 17_666 . . . ?
U2 O3 C5 O7 8.1(9) . . . . ?
U2 O3 C5 C7 -172.0(4) . . . . ?
Si1 C4 C8 C7 -175.9(4) . . . . ?
O3 C5 C7 C6 176.2(6) . . . . ?
O3 C5 C7 C8 -4.7(9) . . . . ?
O7 C5 C7 C6 -3.9(9) . . . . ?
O7 C5 C7 C8 175.2(6) . . . . ?
O9 C1 C2 C3 18.4(10) . . . . ?
O9 C1 C2 C6 -157.5(7) . . . . ?
O10 C1 C2 C3 -161.9(6) . . . . ?
O10 C1 C2 C6 22.2(10) . . . . ?
C1 C2 C3 C4 -178.1(6) . . . . ?
C1 C2 C6 C7 175.9(6) . . . . ?
C2 C3 C4 Si1 178.2(5) . . . . ?
C2 C3 C4 C8 2.2(9) . . . . ?
C2 C6 C7 C5 -178.7(6) . . . . ?
C2 C6 C7 C8 2.2(9) . . . . ?
C3 C2 C6 C7 -0.1(9) . . . . ?
C3 C4 C8 C7 -0.1(9) . . . . ?
C4 Si1 C4 C3 -64.9(4) 19_576 . . . ?
C4 Si1 C4 C3 174.4(5) 28_656 . . . ?
C4 Si1 C4 C3 54.7(4) 10_564 . . . ?
C4 Si1 C4 C8 -9.9(5) 28_656 . . . ?
C4 Si1 C4 C8 110.8(6) 19_576 . . . ?
C4 Si1 C4 C8 -129.6(6) 10_564 . . . ?
C5 C7 C8 C4 178.9(5) . . . . ?
C6 C2 C3 C4 -2.2(10) . . . . ?
C6 C7 C8 C4 -2.1(9) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.836 -0.709 -0.523 5203.4 1575.8 ?
2 -0.879 -0.475 -0.198 5203.4 1470.1 ?
