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_1569299
_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 Cl N2 Np O'
_chemical_formula_sum            'C46 H54 Cl N2 Np O'
_chemical_formula_weight         923.36
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-01-27 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                78.952(12)
_cell_angle_beta                 73.607(15)
_cell_angle_gamma                69.594(13)
_cell_formula_units_Z            2
_cell_length_a                   10.8086(18)
_cell_length_b                   13.8161(17)
_cell_length_c                   17.097(3)
_cell_measurement_reflns_used    4970
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.9050
_cell_measurement_theta_min      1.9300
_cell_volume                     2283.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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    -29.40 135.60   1.00   50.00    --  -11.10  73.75 118.26  165
  2  \w    -29.40 135.60   1.00   50.00    --  -11.10  73.75 -25.74  165
  3  \w    -29.40 135.60   1.00   50.00    --  -11.10  73.75-169.74  165
  4  \w    -29.40 135.60   1.00   50.00    --  -11.10  73.75  46.26  165
  5  \w    -29.40 135.60   1.00   50.00    --  -11.10  73.75 -97.74  165
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0494140000
_diffrn_orient_matrix_UB_12      -0.0190660000
_diffrn_orient_matrix_UB_13      0.0293981000
_diffrn_orient_matrix_UB_21      0.0409936000
_diffrn_orient_matrix_UB_22      -0.0135733000
_diffrn_orient_matrix_UB_23      0.0287676000
_diffrn_orient_matrix_UB_31      -0.0326291000
_diffrn_orient_matrix_UB_32      0.0498527000
_diffrn_orient_matrix_UB_33      0.0140953000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1897
_diffrn_reflns_av_unetI/netI     0.1705
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30922
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.068
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_preparation       'By JM.'
_exptl_crystal_recrystallization_method 'From Et2O at -35C.'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.858
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8223
_refine_ls_number_restraints     318
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0722
_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^)+(0.0601P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4961
_reflns_number_total             8223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02194g2.cif
_cod_data_source_block           1_Np
_cod_depositor_comments
'Adding full bibliography for 1569298--1569306.cif.'
_cod_original_cell_volume        2283.2(7)
_cod_database_code               1569299
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Np Cl2 K C40 N2 O '
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.798
_reflns_odcompleteness_completeness 97.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 2A
3.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C37(H37), C40(H40)
3.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C23(H23), C22(H22), C21(H21), C34(H34), C35(H35),
  C33(H33)
3.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C18(C13,C14,C15,C16,C17), C23(C22,C21,C20,C19,C24),
 C34(C35,C36,C31,C32,C33)
3.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C)
;
_shelx_res_checksum              39091
_shelx_fab_checksum              1859
_platon_squeeze_void_probe_radius 1.20
_lanl_internal_coll_client       JM/LMS/AJG
_lanl_internal_coll_date         12/17/20
_lanl_internal_coll_frame_method '\w scans'
_lanl_internal_coll_frame_time   50s
_lanl_internal_coll_frame_width  1.0
_lanl_internal_coll_name         ms0495
_lanl_internal_coll_type         custom
_lanl_internal_coll_user         CAPG
_lanl_internal_process_date      12/18/20
_lanl_internal_process_user      CAPG
_lanl_internal_refinement_date   2/24/21
_lanl_internal_refinement_user   CAPG
_lanl_internal_solution_date     12/18/20
_lanl_internal_solution_user     CAPG
_olex2_exptl_crystal_mounting_method
'From NVH oil, mounted into a quartz capillary that was sealed at both ends with capillary wax. The outside was then coated with Tough As Nails clear nail varnish to provide shatter resistance.'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.473
_oxdiff_exptl_absorpt_empirical_full_min 0.366