Synthesis and comparison of iso-structural f-block metal complexes (Ce, U, Np, Pu) featuring <i>η</i><sup>6</sup>-arene interactions.
Murillo, Jesse; Goodwin, Conrad A. P.; Stevens, Lauren; Fortier, Skye; Gaunt, Andrew J.; Scott, Brian L.; Chemical science 14 (2023) 7438–7446; doi:10.1039/d3sc02194g

data_1569305
_publ_section_title
;
 Synthesis and comparison of iso-structural f-block metal complexes (Ce,
 U, Np, Pu) featuring <i>&#x3b7;</i><sup>6</sup>-arene interactions.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              7438
_journal_page_last               7446
_journal_paper_doi               10.1039/d3sc02194g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C46 H54 I N2 O U, 0.8(C4 H8 O), 0.2(C4 H10 O)'
_chemical_formula_sum            'C50 H62.4 I N2 O2 U'
_chemical_formula_weight         1088.35
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-11-01
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.8970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7779(8)
_cell_length_b                   15.6184(10)
_cell_length_c                   21.8752(13)
_cell_measurement_reflns_used    9617
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.529
_cell_measurement_theta_min      2.450
_cell_volume                     4479.5(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            134834
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.560
_diffrn_reflns_theta_min         1.957
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.353
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1030 before and 0.0466 after correction. The Ratio of minimum to maximum transmission is 0.7228. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             2150
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00015(2)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         13721
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0161
_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^)+(0.0108P)^2^+4.7647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0353
_refine_ls_wR_factor_ref         0.0362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12929
_reflns_number_total             13721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02194g2.cif
_cod_data_source_block           3_U
_cod_depositor_comments
'Adding full bibliography for 1569298--1569306.cif.'
_cod_original_formula_sum        'C50 H62.40 I N2 O2 U'
_cod_database_code               1569305
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.476
_shelx_estimated_absorpt_t_min   0.476
_olex2_refinement_description
;
1. Restrained distances
 C76-C3 \\sim O56-C5
 with sigma of 0.02
2. Others
 Fixed Sof: O56(0.8) C76(0.8) H76A(0.8) H76B(0.8) C3(0.8) H3A(0.8) H3B(0.8)
 C4(0.8) H4A(0.8) H4B(0.8) C5(0.8) H5A(0.8) H5B(0.8) O0AA(0.2) C1AA(0.2)
 H1AA(0.2) H1AB(0.2) C2AA(0.2) H2AA(0.2) H2AB(0.2) H2AC(0.2) C3AA(0.2)
 H3AA(0.2) H3AB(0.2) H3AC(0.2) C0AA(0.2) H0AA(0.2) H0AB(0.2)
3.a Ternary CH refined with riding coordinates:
 C9(H9), C16(H16), C32(H32), C48(H48)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C40(H40A,H40B), C57(H57A,H57B), C76(H76A,
 H76B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C1AA(H1AA,H1AB), C0AA(H0AA,H0AB)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C21(H21), C23(H23), C24(H24), C27(H27), C28(H28), C35(H35),
 C36(H36), C37(H37), C41(H41), C43(H43), C46(H46), C47(H47), C49(H49), C58(H58),
  C61(H61), C65(H65), C79(H79)
3.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C54(H54A,H54B,
 H54C), C59(H59A,H59B,H59C), C70(H70A,H70B,H70C), C1(H1A,H1B,H1C), C2(H2A,H2B,
 H2C), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC)
;
_shelx_res_checksum              78717
_olex2_submission_special_instructions 'No special instructions were received'