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_7129571
_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_formula_moiety         '2(C50 H58 N2 O24 S2 U2), C2 H6 O S, H2 O'
_chemical_formula_sum            'C102 H124 N4 O50 S5 U4'
_chemical_formula_weight         3318.46
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-03
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2021-11-03 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                   12.89840(10)
_cell_length_b                   21.5255(3)
_cell_length_c                   42.4726(4)
_cell_measurement_reflns_used    36000
_cell_measurement_temperature    100.03(10)
_cell_measurement_theta_max      76.3130
_cell_measurement_theta_min      2.9300
_cell_volume                     11792.3(2)
_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      100.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -55.00  19.00   0.50    7.00    --  -38.50  96.00 134.00  148
  2  \w     51.00  77.00   0.50    7.00    --   42.50 -96.00  25.00   52
  3  \w     63.00 106.00   0.50   28.00    --  111.00 -96.00  25.00   86
  4  \w    124.00 150.00   0.50   28.00    --  111.00  96.00 134.00   52
  5  \w   -107.00 -15.00   0.50    7.00    --  -38.50 -57.00  60.00  184
  6  \w    -40.00  10.00   0.50    7.00    --  -38.50  38.00-120.00  100
  7  \w     57.00  98.00   0.50    7.00    --   42.50-125.00 -60.00   82
  8  \w     17.00 113.00   0.50    7.00    --   42.50  57.00 -90.00  192
  9  \w    -30.00  65.00   0.50    7.00    --   42.50 -38.00 -60.00  190
 10  \w    117.00 158.00   0.50   28.00    --  111.00 125.00-120.00   82
 11  \w    152.00 178.00   0.50   28.00    --  111.00  77.00 -90.00   52
 12  \w     39.00  66.00   0.50   28.00    --  111.00-125.00   0.00   54
 13  \w     47.00 107.00   0.50   28.00    --  111.00 -77.00  30.00  120
 14  \w     43.00  99.00   0.50   28.00    --  111.00-125.00 -30.00  112
 15  \w     38.00  72.00   0.50   28.00    --  111.00 -94.00 -30.00   68
 16  \w    100.00 138.00   0.50   28.00    --  111.00 125.00   0.00   76
 17  \w     51.00 107.00   0.50   28.00    --  111.00 -94.00 120.00  112
 18  \w    120.00 154.00   0.50   28.00    --  111.00  77.00 120.00   68
 19  \w     87.00 176.00   0.50   28.00    --  111.00  45.00-180.00  178
 20  \w     76.00 111.00   0.50   28.00    --  111.00-125.00 -60.00   70
 21  \w     67.00 176.00   0.50   28.00    --  111.00  15.00 -60.00  218
 22  \w    103.00 162.00   0.50   28.00    --  111.00 125.00 -30.00  118
 23  \w     36.00 131.00   0.50   28.00    --  111.00 -30.00 -30.00  190
 24  \w     58.00 107.00   0.50   28.00    --  111.00 -94.00-150.00   98
 25  \w    107.00 153.00   0.50   28.00    --  111.00  77.00-150.00   92
 26  \w    118.00 144.00   0.50   28.00    --  111.00  77.00 -90.00   52
 27  \w     76.00 112.00   0.50   28.00    --  111.00-125.00 120.00   72
 28  \w     83.00 112.00   0.50   28.00    --  111.00-125.00   0.00   58
 29  \w     75.00  76.00   0.50   28.00    --  111.00 -94.00 -30.00    2
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0248220000
_diffrn_orient_matrix_UB_12      -0.0691740000
_diffrn_orient_matrix_UB_13      0.0055697000
_diffrn_orient_matrix_UB_21      -0.0377863000
_diffrn_orient_matrix_UB_22      0.0153484000
_diffrn_orient_matrix_UB_23      0.0335137000
_diffrn_orient_matrix_UB_31      -0.1104997000
_diffrn_orient_matrix_UB_32      0.0103462000
_diffrn_orient_matrix_UB_33      -0.0126956000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            107491
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.781
_diffrn_reflns_theta_min         2.301
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.892
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       block
_exptl_crystal_F_000             6448
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.925
_refine_diff_density_min         -1.900
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Flack x determined using 9510 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1536
_refine_ls_number_reflns         24579
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0541P)^2^+45.3924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                22774
_reflns_number_total             24579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06310c2.cif
_cod_data_source_block           1(dmso)2
_cod_database_code               7129571
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.436
_shelx_estimated_absorpt_t_min   0.109
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
S4A \\sim C87A \\sim C88A \\sim S4B \\sim C87B \\sim C88B: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C101 \\sim S5 \\sim O50 \\sim C102: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O10 \\sim S2 \\sim C37 \\sim C38: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 S4A, C87A, C88A, S4B, C87B, C88B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: S4A(0.75) C87A(0.75) H87A(0.75) H87B(0.75) H87C(0.75) C88A(0.75)
 H88A(0.75) H88B(0.75) H88C(0.75) S4B(0.25) C87B(0.25) H87D(0.25) H87E(0.25)
 H87F(0.25) C88B(0.25) H88D(0.25) H88E(0.25) H88F(0.25)
5.a Free rotating group:
 O11(H11A,H11B)
5.b Ternary CH refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68),
  C89(H89), C90(H90), C91(H91), C92(H92), C93(H93)
5.c Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C48(H48A,H48B), C73(H73A,H73B), C98(H98A,H98B)
5.d Me refined with riding coordinates:
 C87A(H87A,H87B,H87C), C88A(H88A,H88B,H88C), C87B(H87D,H87E,H87F), C88B(H88D,
 H88E,H88F)
5.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C27(H27), C28(H28),
 C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C52(H52), C53(H53), C55(H55),
  C56(H56), C57(H57), C58(H58), C61(H61), C77(H77), C78(H78), C80(H80),
 C81(H81), C82(H82), C83(H83), C86(H86)
5.f Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C45(H45A,
 H45B,H45C), C47(H47A,H47B,H47C), C50(H50A,H50B,H50C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C75(H75A,H75B,
 H75C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C), C100(H10A,H10B,H10C),
 C101(H10D,H10E,H10F), C102(H10G,H10H,H10I)
;
_shelx_res_checksum              49366
_shelx_fab_checksum              19990
_olex2_submission_special_instructions 'No special instructions were received'