Enhancing photosensitivity via assembly of a uranyl coordination polymer
Xu, Miaomiao; Lu, Huangjie; Wang, Chunhui; Qiu, Jie; Zheng, Zhaofa; Guo, Xiaofeng; Zhang, Zhi-Hui; He, Mingyang; Qian, Junfeng; Lin, Jian; Chemical Communications  (2022) –; doi:10.1039/D2CC02985E

data_7130396
_publ_section_title
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 Enhancing photosensitivity via assembly of a uranyl coordination polymer
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02985E
_journal_year                    2022
_chemical_formula_moiety         'C12 H9 N5 O5 U, 0.5(H2 O), 0.5(C2 H7 N)'
_chemical_formula_sum            'C13 H13.5 N5.5 O5.5 U'
_chemical_formula_weight         572.82
_chemical_name_common
'Uranyl 2,6-bis(pyrazol-1-yl)pyridine-4-carboxylate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-26
_audit_creation_method
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Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
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_audit_update_record
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2022-05-21 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 93.952(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.813(2)
_cell_length_b                   4.3839(3)
_cell_length_c                   17.693(2)
_cell_measurement_reflns_used    4574
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.8810
_cell_measurement_theta_min      1.9560
_cell_volume                     1610.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -78.10 152.90   0.50    5.00  12.27 -11.30 -28.85    --   462
  2  \w   -106.96  17.54   0.50    5.00    --  -11.30 -59.25  92.08  249
  3  \w   -106.96  17.54   0.50    5.00    --  -11.30 -59.25 164.08  249
;
_diffrn_measurement_device       'Bruker D8-Venture'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0243238000
_diffrn_orient_matrix_UB_12      -0.0867449000
_diffrn_orient_matrix_UB_13      -0.0201611000
_diffrn_orient_matrix_UB_21      0.0225247000
_diffrn_orient_matrix_UB_22      -0.0464573000
_diffrn_orient_matrix_UB_23      -0.0260380000
_diffrn_orient_matrix_UB_31      0.0082954000
_diffrn_orient_matrix_UB_32      -0.1284213000
_diffrn_orient_matrix_UB_33      0.0229988000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18952
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'I\^I1/4S 3.0 microfocus X-ray source'
_diffrn_source_type              'Mo K\a'
_exptl_absorpt_coefficient_mu    10.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.061
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0592P)^2^+25.4282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2262
_reflns_number_total             2836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02985e2.cif
_cod_data_source_block           U-bppCOO
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C13 H13.50 N5.50 O5.50 U'
_cod_database_code               7130396
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O4-U1 = U1-O3
 1.8 with sigma of 0.02
 O4A-U1A = U1A-O3A
 1.8 with sigma of 0.02
 C14-N6 = N6-C13
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O2A)
\\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O4A) \\sim Ueq,
Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O3A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O5A) = Uanis(O5)
Uanis(O4A) = Uanis(O4)
Uanis(O3A) = Uanis(O3)
4. Rigid body (RIGU) restrains
 U1, U1A, O1, O1A, O2, O2A, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 U1, U1A, O1, O1A, O2, O2A, O3, O3A, O4, O4A, O5, O5A, H4, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 U1, U1A, O1, O1A, O2, O2A, O3, O3A, O4, O4A, O5, O5A, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, N6, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(U1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(H5A)=1-FVAR(1)
 Sof(U1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(H5)=FVAR(1)
 Fixed Sof: O6(0.5) H6B(0.5) H6C(0.5) N6(0.5) H6A(0.5) C13(0.5) H13A(0.5)
 H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
6.a Riding coordinates:
 O5(H5), O5A(H5A)
6.b Free rotating group:
 O6(H6B,H6C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), N6(H6A)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
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_shelx_res_checksum              68997
_shelx_hkl_checksum              46227
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.686
_oxdiff_exptl_absorpt_empirical_full_min 0.444