#------------------------------------------------------------------------------
#$Date: 2020-05-28 04:20:59 +0300 (Thu, 28 May 2020) $
#$Revision: 252418 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/81/1558130.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_1558130
loop_
_publ_author_name
'Halter, Dominik P.'
'Klein, Ryan A.'
'Boreen, Michael'
'Trump, Benjamin A.'
'Brown, Craig M.'
'Long, Jeffrey R.'
_publ_section_title
;
 Self-Adjusting Binding Pockets Enhance H2 and CH4 Adsorption in a
 Uranium-Based Metal--Organic Framework
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02394A
_journal_year                    2020
_chemical_formula_moiety         '0.25(C64 H32 O32 U4), 4(O)'
_chemical_formula_sum            'C16 H8 O12 U'
_chemical_formula_weight         630.25
_chemical_name_systematic
'catnea-[bis(?-terephthalato)uranium tetrahydrate]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-11 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.702(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7447(17)
_cell_length_b                   12.5982(12)
_cell_length_c                   9.2934(8)
_cell_measurement_reflns_used    17204
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.095
_cell_measurement_theta_min      2.591
_cell_volume                     1887.4(3)
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON-II CPAD detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17204
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.095
_diffrn_reflns_theta_min         2.591
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_exptl_absorpt_coefficient_mu    4.018
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_description       needle
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.326
_refine_diff_density_min         -1.946
_refine_diff_density_rms         0.325
_refine_ls_extinction_coef       0.0082(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0531
_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)+(0.0966P)²+38.8439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1445
_reflns_number_total             1944
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc02394a2.cif
_cod_data_source_block           1-H2O
_cod_database_code               1558130
_shelx_shelxl_version_number     2014/7
_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   0.980
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C6(H6), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.0000 0.00124(4) 0.2500 0.0152(4) Uani 1 2 d S T P . .
O4 O -0.4465(5) -0.3485(6) -0.5836(8) 0.0276(18) Uani 1 1 d . . . . .
O1 O -0.1310(5) -0.0486(7) 0.0438(7) 0.0269(17) Uani 1 1 d . . . . .
O3 O -0.4764(5) -0.3541(7) -0.3742(9) 0.0313(18) Uani 1 1 d . . . . .
O2 O -0.1012(5) -0.0441(8) -0.1662(9) 0.0307(18) Uani 1 1 d . . . . .
C1 C -0.1490(7) -0.0636(10) -0.1016(12) 0.028(2) Uani 1 1 d . . . . .
C8 C -0.4368(7) -0.3166(10) -0.4492(13) 0.030(3) Uani 1 1 d . . . . .
C2 C -0.2307(6) -0.1140(9) -0.1988(11) 0.022(2) Uani 1 1 d . . . A -2
C5 C -0.3712(6) -0.2369(9) -0.3686(12) 0.022(2) Uani 1 1 d . . . A -2
C4 C -0.3518(7) -0.2095(9) -0.2103(12) 0.027(2) Uani 1 1 d . . . A -2
H4 H -0.3858 -0.2336 -0.1607 0.032 Uiso 1 1 calc R . . A -2
C7 C -0.2545(7) -0.1321(11) -0.3581(12) 0.033(3) Uani 1 1 d . . . A -2
H7 H -0.2237 -0.1011 -0.4101 0.039 Uiso 1 1 calc R . . A -2
C6 C -0.3228(7) -0.1952(9) -0.4434(12) 0.027(2) Uani 1 1 d . . . A -2
H6 H -0.3370 -0.2104 -0.5518 0.032 Uiso 1 1 calc R . . A -2
C3 C -0.2827(7) -0.1470(10) -0.1271(12) 0.030(3) Uani 1 1 d . . . A -2
H3 H -0.2704 -0.1266 -0.0212 0.036 Uiso 1 1 calc R . . A -2
O6 O -0.2608(11) -0.2623(9) -0.3569(16) 0.069(4) Uani 1 1 d . . . A 2
O5 O -0.2400(12) -0.2362(9) -0.1444(16) 0.073(4) Uani 1 1 d . . . B 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.00337 0.00172 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.01151 0.00644 'Calculated using XDISP in WinGX (Farrugia, 1999)'
U U -10.96077 4.15800 'Calculated using XDISP in WinGX (Farrugia, 1999)'
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 O4 74.4(4) 3_556 4_454 ?
O4 U1 O1 136.0(3) 4_454 2 ?
O4 U1 O1 72.4(3) 3_556 2 ?
O4 U1 O1 136.0(3) 3_556 . ?
O4 U1 O1 72.4(3) 4_454 . ?
O1 U1 O1 149.7(4) . 2 ?
O3 U1 O4 148.9(3) 8_546 3_556 ?
O3 U1 O4 114.8(3) 8_546 4_454 ?
O3 U1 O4 114.8(3) 7_445 3_556 ?
O3 U1 O4 148.9(3) 7_445 4_454 ?
O3 U1 O1 73.1(3) 7_445 2 ?
O3 U1 O1 82.6(3) 8_546 2 ?
O3 U1 O1 73.1(3) 8_546 . ?
O3 U1 O1 82.6(3) 7_445 . ?
O3 U1 O3 73.5(4) 8_546 7_445 ?
O2 U1 O4 75.5(3) 5 4_454 ?
O2 U1 O4 75.5(3) 6_556 3_556 ?
O2 U1 O4 82.9(3) 6_556 4_454 ?
O2 U1 O4 82.9(3) 5 3_556 ?
O2 U1 O1 115.1(3) 6_556 2 ?
O2 U1 O1 115.1(3) 5 . ?
O2 U1 O1 72.5(3) 6_556 . ?
O2 U1 O1 72.5(3) 5 2 ?
O2 U1 O3 133.4(3) 6_556 8_546 ?
O2 U1 O3 71.9(3) 5 8_546 ?
O2 U1 O3 133.4(3) 5 7_445 ?
O2 U1 O3 71.9(3) 6_556 7_445 ?
O2 U1 O2 152.8(5) 5 6_556 ?
C8 O4 U1 139.0(7) . 3_444 ?
C1 O1 U1 128.3(7) . . ?
C8 O3 U1 146.1(8) . 7_445 ?
C1 O2 U1 171.9(7) . 5 ?
O1 C1 C2 117.2(9) . . ?
O2 C1 O1 124.3(10) . . ?
O2 C1 C2 118.4(9) . . ?
O4 C8 O3 123.4(11) . . ?
O4 C8 C5 118.1(10) . . ?
O3 C8 C5 118.2(10) . . ?
C7 C2 C1 120.2(10) . . ?
C7 C2 C3 119.5(10) . . ?
C3 C2 C1 120.2(9) . . ?
C4 C5 C8 119.4(10) . . ?
C4 C5 C6 119.4(10) . . ?
C6 C5 C8 120.9(9) . . ?
C3 C4 C5 119.6(10) . . ?
C2 C7 C6 120.6(11) . . ?
C2 C7 O6 98.6(10) . . ?
C6 C7 O6 52.2(9) . . ?
C7 C6 C5 119.8(9) . . ?
O6 C6 C5 89.2(10) . . ?
O6 C6 C7 73.7(10) . . ?
C4 C3 C2 120.3(10) . . ?
C6 O6 C7 54.1(7) . . ?
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 2.377(7) 3_556 ?
U1 O4 2.377(7) 4_454 ?
U1 O1 2.398(7) 2 ?
U1 O1 2.398(7) . ?
U1 O3 2.312(8) 7_445 ?
U1 O3 2.312(8) 8_546 ?
U1 O2 2.300(7) 6_556 ?
U1 O2 2.300(7) 5 ?
O4 U1 2.377(7) 3_444 ?
O4 C8 1.254(13) . ?
O1 C1 1.266(12) . ?
O3 U1 2.312(8) 7_445 ?
O3 C8 1.269(14) . ?
O2 U1 2.300(7) 5 ?
O2 C1 1.251(13) . ?
C1 C2 1.492(15) . ?
C8 C5 1.483(15) . ?
C2 C7 1.379(14) . ?
C2 C3 1.407(14) . ?
C5 C4 1.406(14) . ?
C5 C6 1.411(15) . ?
C4 C3 1.389(16) . ?
C7 C6 1.389(16) . ?
C7 O6 1.645(18) . ?
C6 O6 1.354(17) . ?
