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_1569303
_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 Ce I N2 O, C4 H10 O'
_chemical_formula_sum            'C50 H64 Ce I N2 O2'
_chemical_formula_weight         992.05
_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             2022-10-27
_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                 98.817(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4528(4)
_cell_length_b                   21.5419(9)
_cell_length_c                   18.1661(7)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.21
_cell_volume                     4428.9(3)
_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 0.998
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            75264
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.557
_diffrn_reflns_theta_min         2.033
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0782 before and 0.0579 after correction. The Ratio of minimum to maximum transmission is 0.9046. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       needle
_exptl_crystal_F_000             2020
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.725
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         13549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+0.9560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10781
_reflns_number_total             13549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02194g2.cif
_cod_data_source_block           3_Ce
_cod_depositor_comments
'Adding full bibliography for 1569298--1569306.cif.'
_cod_database_code               1569303
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.332
_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:
 C00Q(H00Q), C00V(H00V), C00Z(H00Z), C011(H011)
2.b Secondary CH2 refined with riding coordinates:
 C010(H01A,H01B), C016(H01F,H01G), C01A(H01K,H01L), C01G(H01Z,HB), C01H(H01,
 HC), C01K(H2AA,HH)
2.c Aromatic/amide H refined with riding coordinates:
 C007(H007), C008(H008), C00A(H00A), C00F(H00F), C00J(H00J), C00M(H00M),
 C00O(H00O), C00P(H00P), C00R(H00R), C00T(H00T), C00U(H00U), C00X(H00X),
 C00Y(H00Y), C012(H012), C013(H013), C014(H014), C017(H017), C018(H018)
2.d Idealised Me refined as rotating group:
 C00S(H00B,H00C,H00D), C015(H01C,H01D,H01E), C019(H01H,H01I,H01J), C01B(H01M,
 H01N,H01O), C01C(H01P,H01Q,H01R), C01D(H01S,H01T,H01U), C01E(H01V,H01W,H01X),
 C01F(H01Y,H,HA), C01I(H0AA,HD,HE), C01J(H1AA,HF,HG)
;
_shelx_res_checksum              2941
_olex2_submission_special_instructions 'No special instructions were received'