Insights at the molecular level into the formation of oxo-bridged trinuclear uranyl complexes
Schaper, Gerrit; Wenzel, Marco; Schwarzenbolz, Uwe; Steup, Johannes; Hennersdorf, Felix; Henle, Thomas; Lindoy, Leonard F.; Weigand, Jan J.; Chemical Communications  (2022) –; doi:10.1039/D1CC06310C

data_7129570
_publ_section_title
;
 Insights at the molecular level into the formation of oxo-bridged
 trinuclear uranyl complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06310C
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H27 N O10'
_chemical_formula_sum            'C22 H27 N O10'
_chemical_formula_weight         465.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2022-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.74940(10)
_cell_length_b                   14.25760(10)
_cell_length_c                   28.6021(3)
_cell_measurement_reflns_used    7401
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4040
_cell_measurement_theta_min      3.4510
_cell_volume                     2344.59(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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    -79.00  -1.00   0.50    0.50    --  -38.50 109.00 149.00  156
  2  \w    -19.00   8.00   0.50    0.50    --   42.62 -74.00 -62.00   54
  3  \w    115.00 156.00   0.50    1.00    --  111.00  74.00  65.00   82
  4  \w     64.00 115.00   0.50    1.00    --  111.00 -50.00 134.00  102
  5  \w     50.00  78.00   0.50    1.00    --  111.00-109.00  52.00   56
  6  \w    -55.00  -6.00   0.50    0.50    --  -38.50 125.00-180.00   98
  7  \w    -87.00  -6.00   0.50    0.50    --  -38.50 125.00 -60.00  162
  8  \w     36.00 115.00   0.50    1.00    --  111.00 -30.00 -60.00  158
  9  \w     42.00 141.00   0.50    1.00    --  111.00 -77.00 150.00  198
 10  \w     98.00 175.00   0.50    1.00    --  111.00 125.00  90.00  154
 11  \w     68.00  95.00   0.50    1.00    --  111.00-125.00  30.00   54
 12  \w     88.00 178.00   0.50    1.00    --  111.00  30.00   0.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            10772
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.627
_diffrn_reflns_theta_min         3.090
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 1881 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+0.1257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.710
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                4676
_reflns_number_total             4828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06310c2.cif
_cod_data_source_block           ii
_cod_database_code               7129570
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C8(H8), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21)
2.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C),
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              69568
_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
;