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_1569304
_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 Pu, 0.67(C4 H8 O), 0.33(C4 H10 O)'
_chemical_formula_sum            'C50 H62.67 I N2 O2 Pu'
_chemical_formula_weight         1092.58
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     dual
_audit_creation_date             2022-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.057(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8050(10)
_cell_length_b                   15.6334(12)
_cell_length_c                   21.9877(18)
_cell_measurement_reflns_used    9642
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.46
_cell_volume                     4511.6(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78010
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.332
_diffrn_reflns_theta_min         2.026
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1693 before and 0.0879 after correction. The Ratio of minimum to maximum transmission is 0.5446. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       needle
_exptl_crystal_F_000             2159
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.837
_refine_diff_density_min         -2.460
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.00040(8)
_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   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         11214
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+10.8321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9488
_reflns_number_total             11214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02194g2.cif
_cod_data_source_block           3_Pu
_cod_depositor_comments
'Adding full bibliography for 1569298--1569306.cif.'
_cod_database_code               1569304
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.310
_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. Rigid bond restraints
 C16, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, C16, C17, C18, C14, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C14 \\sim C13 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C18 \\sim C13: within 0.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C13 \\sim C18: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C16 \\sim C15: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C17 \\sim C16: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
C14 \\sim C15: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
4. Others
 Fixed Sof: O2(0.66666) C49(0.66666) H49A(0.66666) H49B(0.66666) C47(0.66666)
 H47A(0.66666) H47B(0.66666) C48(0.66666) H48A(0.66666) H48B(0.66666)
 C50(0.66666) H50A(0.66666) H50B(0.66666) C54(0.33333) H54A(0.33333)
 H54B(0.33333) H54C(0.33333) O3(0.33333) C53(0.33333) H53A(0.33333)
 H53B(0.33333) C51(0.33333) H51A(0.33333) H51B(0.33333) H51C(0.33333)
 C52(0.33333) H52A(0.33333) H52B(0.33333)
5.a Ternary CH refined with riding coordinates:
 C40(H40), C37(H37), C28(H28), C25(H25)
5.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C43(H43A,H43B), C45(H45A,H45B), C44(H44A,H44B), C49(H49A,
 H49B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B), C53(H53A,H53B),
 C52(H52A,H52B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C12(H12), C9(H9), C3(H3), C5(H5), C33(H33), C11(H11), C10(H10),
 C35(H35), C2(H2), C34(H34), C22(H22), C23(H23), C21(H21), C15(H15), C18(H18),
 C16(H16), C17(H17)
5.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C27(H27A,
 H27B,H27C), C54(H54A,H54B,H54C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              21072
_olex2_submission_special_instructions 'No special instructions were received'