An anionic potassium-organic framework for selective removal of uranyl ions.
Yang, Qianqian; Wang, Yijie; Yang, Jianjian; Yin, Jianbo; Liu, Di; Liu, Ning; Wang, Rongming; Sun, Daofeng; Li, Xiyou; Jiang, Jianzhuang; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8314–8321; doi:10.1039/d1dt00822f

data_7707329
_publ_section_title
;
 An anionic potassium-organic framework for selective removal of uranyl
 ions.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8314
_journal_page_last               8321
_journal_paper_doi               10.1039/d1dt00822f
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C54 H34 K O8, C2 H8 N'
_chemical_formula_sum            'C56 H42 K N O8'
_chemical_formula_weight         896.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-24 deposited with the CCDC.	2021-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2471(2)
_cell_length_b                   43.0335(8)
_cell_length_c                   10.3618(2)
_cell_measurement_reflns_used    7492
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.4980
_cell_measurement_theta_min      4.1050
_cell_volume                     4569.23(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -24.00   5.00   1.00    1.00    --    0.00  73.00 130.00   29
  2  \w    -39.00 -13.00   1.00    1.00    --    0.00 -73.00   1.00   26
  3  \w     48.00  76.00   1.00    2.50    --   54.00 -73.00   1.00   28
  4  \w     70.00 124.00   1.00    2.50    --   54.00  73.00 130.00   54
  5  \w    123.00 154.00   1.00    5.00    --  108.00  73.00 130.00   31
  6  \w     68.00 131.00   1.00    5.00    --  108.00 -73.00   1.00   63
  7  \w     28.00  69.00   1.00    1.00    --    0.00  57.00-180.00   41
  8  \w     42.00  99.00   1.00    2.50    --   54.00  57.00-120.00   57
  9  \w     23.00  99.00   1.00    2.50    --   54.00-125.00  30.00   76
 10  \w     53.00  96.00   1.00    5.00    --  108.00-111.00-120.00   43
 11  \w     35.00 111.00   1.00    5.00    --  108.00-111.00  30.00   76
 12  \w     86.00 113.00   1.00    5.00    --  108.00  63.00-150.00   27
 13  \w    149.00 175.00   1.00    5.00    --  108.00  63.00-150.00   26
 14  \w    108.00 173.00   1.00    5.00    --  108.00  63.00  90.00   65
 15  \w     35.00  69.00   1.00    5.00    --  108.00-111.00 -60.00   34
 16  \w     29.00  69.00   1.00    1.00    --    0.00  57.00 -90.00   40
 17  \w    -20.00   6.00   1.00    1.00    --    0.00  57.00 120.00   26
 18  \w     31.00  60.00   1.00    1.00    --    0.00  57.00 120.00   29
 19  \w     72.00 114.00   1.00    2.50    --   54.00  38.00  90.00   42
 20  \w     44.00  74.00   1.00    2.50    --   54.00 -57.00  30.00   30
 21  \w     13.00  65.00   1.00    2.50    --   54.00 -99.00-180.00   52
 22  \w     81.00 121.00   1.00    2.50    --   54.00  57.00-180.00   40
 23  \w     71.00  97.00   1.00    2.50    --   54.00 -99.00-180.00   26
 24  \w    -14.00  28.00   1.00    2.50    --   54.00 -57.00 -90.00   42
 25  \w     41.00  69.00   1.00    2.50    --   54.00 -57.00 -90.00   28
 26  \w     37.00  63.00   1.00    2.50    --   54.00  38.00-180.00   26
 27  \w    -15.00  23.00   1.00    2.50    --   54.00 -57.00  30.00   38
 28  \w    117.00 151.00   1.00    5.00    --  108.00 178.00 -90.00   34
 29  \w     60.00 102.00   1.00    5.00    --  108.00 178.00 -90.00   42
 30  \w     87.00 175.00   1.00    5.00    --  108.00  63.00  30.00   88
 31  \w     36.00 109.00   1.00    5.00    --  108.00-111.00 -90.00   73
 32  \w    109.00 140.00   1.00    5.00    --  108.00 -77.00-180.00   31
 33  \w    116.00 157.00   1.00    5.00    --  108.00  63.00-120.00   41
 34  \w     93.00 155.00   1.00    5.00    --  108.00  63.00   0.00   62
 35  \w     38.00  66.00   1.00    5.00    --  108.00 -77.00-180.00   28
 36  \w     43.00 130.00   1.00    5.00    --  108.00 -63.00 -60.00   87
 37  \w     84.00 110.00   1.00    5.00    --  108.00-111.00 120.00   26
 38  \w     81.00 106.00   1.00    5.00    --  108.00-111.00 -60.00   25
 39  \w     67.00 124.00   1.00    5.00    --  108.00 -50.00   0.00   57
 40  \w    124.00 168.00   1.00    5.00    --  108.00  50.00 -60.00   44
 41  \w     89.00 115.00   1.00    5.00    --  108.00  50.00 -60.00   26
 42  \w    125.00 169.00   1.00    5.00    --  108.00 111.00 -90.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0082770000
_diffrn_orient_matrix_UB_12      -0.0116727000
_diffrn_orient_matrix_UB_13      0.1403376000
_diffrn_orient_matrix_UB_21      0.0915027000
_diffrn_orient_matrix_UB_22      -0.0264252000
_diffrn_orient_matrix_UB_23      -0.0431875000
_diffrn_orient_matrix_UB_31      0.1189519000
_diffrn_orient_matrix_UB_32      0.0211496000
_diffrn_orient_matrix_UB_33      0.0235051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.527
_diffrn_reflns_theta_min         4.435
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.494
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1684 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4351
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0424
_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/[\s^2^(Fo^2^)+(0.0917P)^2^+1.1223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                4104
_reflns_number_total             4351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00822f2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7707329.cif.'
_cod_database_code               7707329
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.754
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H2A-O2
 0.85 with sigma of 0.01
 C28-C29
 2.4 with sigma of 0.02
 C28-N1 = N1-C29
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C29) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N1, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C15(H15), C18(H18), C21(H21), C26(H26), C27(H27)
6.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              15118
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.479
_oxdiff_exptl_absorpt_empirical_full_min 0.723