Single crystal structure and photocatalytic behavior of grafted uranyl on the Zr-node of a pyrene-based metal‒organic framework
Knapp, Julia G.; Zhang, Xuan; Elkin, Tatyana; Wolfsberg, Laura E.; Hanna, Sylvia L.; Son, Florencia A.; Scott, Brian L.; Farha, Omar K.; CrystEngComm  (2020) –; doi:10.1039/C9CE02034A

data_7239996
_publ_section_title
;
 Single crystal structure and photocatalytic behavior of grafted uranyl on
 the Zr-node of a pyrene-based metal--organic framework
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE02034A
_journal_year                    2020
_chemical_formula_moiety         '0.17(C264 H132 O97.8 U1.61 Zr18)'
_chemical_formula_sum            'C44 H22 O16.3 U0.27 Zr3'
_chemical_formula_weight         1148.95
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-13 deposited with the CCDC.	2020-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   39.5261(3)
_cell_length_b                   39.5261(3)
_cell_length_c                   16.52780(10)
_cell_measurement_reflns_used    49065
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      67.9070
_cell_measurement_theta_min      2.2270
_cell_volume                     22362.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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      200(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.985
_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    184.92 304.92   0.50   50.00    --  -97.00-149.49 -10.01  240
  2  \w    199.52 321.52   0.50   50.00    --  -98.00-174.45 159.96  244
  3  \f     16.90 270.90   0.50   10.00  71.60  56.00-144.49    --   508
  4  \w    180.95 283.95   0.50   50.00    -- -100.00-114.50  45.00  206
  5  \f   -334.48   9.02   0.50    5.00  10.35   8.00  30.50    --   687
  6  \w     69.02 127.52   0.50   10.00    --   42.00 130.49 -45.00  117
  7  \f   -105.96   9.04   0.50   49.98-124.30-100.00 -44.49    --   230
  8  \w    -34.48  65.52   0.50    5.00    --  -20.00  70.50 -25.00  200
  9  \w    -11.09  38.41   0.50   10.00    --   36.00 -29.49   9.99   99
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0155150000
_diffrn_orient_matrix_UB_12      0.0237017000
_diffrn_orient_matrix_UB_13      -0.0446647000
_diffrn_orient_matrix_UB_21      0.0031717000
_diffrn_orient_matrix_UB_22      -0.0173860000
_diffrn_orient_matrix_UB_23      -0.0811642000
_diffrn_orient_matrix_UB_31      -0.0421237000
_diffrn_orient_matrix_UB_32      -0.0340812000
_diffrn_orient_matrix_UB_33      0.0103480000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            98944
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.137
_diffrn_reflns_theta_min         2.236
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.680
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.512
_exptl_crystal_description       needle
_exptl_crystal_F_000             3367
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.141
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         7483
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0542
_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/[\s^2^(Fo^2^)+(0.1445P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.1916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6350
_reflns_number_total             7483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce02034a2.cif
_cod_data_source_block           xz156
_cod_original_cell_volume        22362.1(4)
_cod_original_formula_sum        'C44 H22 O16.30 U0.27 Zr3'
_cod_database_code               7239996
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.739
_reflns_odcompleteness_completeness 98.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.02
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 U1-O7
 2.67 with sigma of 0.02
 Zr2-O4
 2.247 with sigma of 0.02
 Zr1-O4
 2.3 with sigma of 0.02
 Zr1-O3A
 2.3 with sigma of 0.02
 Zr2-O3A
 2.23 with sigma of 0.02
 U2-O3A
 2.83 with sigma of 0.02
 U4-O4
 2.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O8) = Uanis(O7)
Uanis(O4) = Uanis(O4A)
Uanis(O3) = Uanis(O3A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O3A)=0.5*(1-FVAR(2))
 Sof(O3)=0.5*FVAR(2)
 Sof(O4)=0.5*(1-FVAR(3))
 Sof(O4A)=0.5*FVAR(3)
 Fixed Sof: U1(0.025) U3(0.02) O8(0.05) U2(0.007) O7(0.025) U4(0.015)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C9(H9), C4(H4), C6(H6), C12(H12)
;
_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 1.597
_oxdiff_exptl_absorpt_empirical_full_min 0.537