2.2.2-Cryptand complexes of neptunium(iii) and plutonium(iii)
Goodwin, Conrad A. P.; Ciccone, Sierra R.; Bekoe, Samuel; Majumdar, Sourav; Scott, Brian L.; Ziller, Joseph W.; Gaunt, Andrew J.; Furche, Filipp; Evans, William J.; Chemical Communications  (2022) –; doi:10.1039/D1CC05904A

data_7129460
_publ_section_title
;
 2.2.2-Cryptand complexes of neptunium(iii) and plutonium(iii)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05904A
_journal_year                    2022
_chemical_formula_moiety         'C20 H36 F6 N2 O12 Pu S2, C F3 O3 S'
_chemical_formula_sum            'C21 H36 F9 N2 O15 Pu S3'
_chemical_formula_weight         1062.76
_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             2021-04-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-10 deposited with the CCDC.	2021-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                64.334(16)
_cell_angle_beta                 64.496(16)
_cell_angle_gamma                62.224(17)
_cell_formula_units_Z            6
_cell_length_a                   18.231(3)
_cell_length_b                   19.555(3)
_cell_length_c                   19.607(3)
_cell_measurement_reflns_used    6903
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.1100
_cell_measurement_theta_min      1.9370
_cell_volume                     5340.2(18)
_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)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_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      2.26 122.26   0.50    3.00    --   28.00  73.75 -25.74  240
  2  \w      2.26 122.26   0.50    3.00    --   28.00  73.75  64.26  240
  3  \w    -53.74  65.76   0.50    3.00    --  -28.00  73.75 154.26  239
  4  \w    -53.74  65.76   0.50    3.00    --  -28.00  73.75-115.74  239
;
_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      0.0206720000
_diffrn_orient_matrix_UB_12      0.0279070000
_diffrn_orient_matrix_UB_13      -0.0114295000
_diffrn_orient_matrix_UB_21      0.0026073000
_diffrn_orient_matrix_UB_22      -0.0130148000
_diffrn_orient_matrix_UB_23      0.0389968000
_diffrn_orient_matrix_UB_31      0.0408968000
_diffrn_orient_matrix_UB_32      -0.0297986000
_diffrn_orient_matrix_UB_33      -0.0101910000
_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  0.0831
_diffrn_reflns_av_unetI/netI     0.1084
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43582
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.955
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18422
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_description       plate
_exptl_crystal_F_000             3114
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From THF layered with Et2O at -35C.'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.317
_refine_diff_density_min         -1.718
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1479
_refine_ls_number_reflns         20091
_refine_ls_number_restraints     3824
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0657
_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^)+(0.0895P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13617
_reflns_number_total             20091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05904a2.cif
_cod_data_source_block           ms0608
_cod_original_cell_volume        5340.4(19)
_cod_database_code               7129460
_lanl_internal_coll_name         ms0608
_lanl_internal_coll_client       CAPG
_lanl_internal_coll_type         custom
_lanl_internal_coll_frame_time   3s
_lanl_internal_coll_frame_width  0.5
_lanl_internal_coll_frame_method '\w scans'
_lanl_internal_coll_user         CAPG
_lanl_internal_coll_date         04/22/21
_lanl_internal_process_user      CAPG
_lanl_internal_process_date      04/22/21
_lanl_internal_solution_user     CAPG
_lanl_internal_solution_date     04/27/21
_lanl_internal_refinement_user   CAPG
_lanl_internal_refinement_date   04/27/21
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C21H36F9N2O15PuS3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.674
_reflns_odcompleteness_completeness 98.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 F1-F2 \\sim F2-F3 \\sim F1-F3 \\sim F4-F5 \\sim F5-F6 \\sim F4-F6 \\sim F7-F8
\\sim F8-F9 \\sim F7-F9 \\sim F10-
 F11 \\sim F11-F12 \\sim F10-F12 \\sim F13-F14 \\sim F14-F15 \\sim F13-F15
\\sim F16A-F17A \\sim F17A-F18A
 \\sim F16A-F18A \\sim F16B-F17B \\sim F17B-F18B \\sim F16B-F18B \\sim F19-F20
\\sim F20-F21 \\sim F19-F21
 \\sim F22A-F23A \\sim F23A-F24A \\sim F22A-F24A \\sim F22B-F23B \\sim
F23B-F24B \\sim F22B-F24B \\sim F25-
 F26 \\sim F26-F27 \\sim F25-F27
 with sigma of 0.005
 F1-C19 \\sim F2-C19 \\sim F3-C19 \\sim F4-C20 \\sim F5-C20 \\sim F6-C20 \\sim
F7-C21 \\sim F8-C21 \\sim F9-
 C21 \\sim F10-C40 \\sim F11-C40 \\sim F12-C40 \\sim F13-C41 \\sim F14-C41
\\sim F15-C41 \\sim F16A-C42A ~
 F17A-C42A \\sim F18A-C42A \\sim F16B-C42B \\sim F17B-C42B \\sim F18B-C42B
\\sim F19-C61 \\sim F20-C61
 \\sim F21-C61 \\sim F22A-C62A \\sim F23A-C62A \\sim F24A-C62A \\sim F22B-C62B
\\sim F23B-C62B \\sim F24B-
 C62B \\sim F25-C63 \\sim F26-C63 \\sim F27-C63
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.008 and sigma
for terminal atoms of 0.008 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
5. Others
 Sof(S8B)=Sof(O42B)=Sof(C62B)=Sof(F24B)=Sof(F23B)=Sof(F22B)=Sof(O41B)=1-FVAR(1)
 Sof(S8A)=Sof(F23A)=Sof(F24A)=Sof(O42A)=Sof(F22A)=Sof(C62A)=Sof(O41A)=FVAR(1)
 Sof(F18B)=Sof(F17B)=Sof(F16B)=Sof(C42B)=1-FVAR(2)
 Sof(C42A)=Sof(F16A)=Sof(F18A)=Sof(F17A)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C36(H36A,H36B), C37(H37A,H37B), C44(H44A,H44B), C33(H33A,
 H33B), C23(H23A,H23B), C45(H45A,H45B), C46(H46A,H46B), C35(H35A,H35B),
 C57(H57A,H57B), C2(H2A,H2B), C43(H43A,H43B), C16(H16A,H16B), C27(H27A,H27B),
 C34(H34A,H34B), C10(H10A,H10B), C3(H3A,H3B), C58(H58A,H58B), C29(H29A,H29B),
 C50(H50A,H50B), C51(H51A,H51B), C56(H56A,H56B), C49(H49A,H49B), C5(H5A,H5B),
 C18(H18A,H18B), C39(H39A,H39B), C17(H17A,H17B), C32(H32A,H32B), C31(H31A,H31B),
  C15(H15A,H15B), C7(H7A,H7B), C9(H9A,H9B), C47(H47A,H47B), C12(H12A,H12B),
 C55(H55A,H55B), C30(H30A,H30B), C13(H13A,H13B), C1(H1A,H1B), C22(H22A,H22B),
 C8(H8A,H8B), C11(H11A,H11B), C48(H48A,H48B), C38(H38A,H38B), C54(H54A,H54B),
 C28(H28A,H28B), C4(H4A,H4B), C6(H6A,H6B), C25(H25A,H25B), C14(H14A,H14B),
 C52(H52A,H52B), C24(H24A,H24B), C59(H59A,H59B), C60(H60A,H60B), C53(H53A,H53B)
;
_shelx_res_checksum              65869
_olex2_exptl_crystal_mounting_method
'From NVH oil into a quartz capillary which was sealed at both ends with capilllary wax. The outside was then coated in 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 5.882
_oxdiff_exptl_absorpt_empirical_full_min 0.449