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_7129459
_publ_section_title
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 2.2.2-Cryptand complexes of neptunium(iii) and plutonium(iii)
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05904A
_journal_year                    2022
_chemical_formula_sum            'C21 H36 F9 N2 O15 S3 U'
_chemical_formula_weight         1061.73
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-09-10 deposited with the CCDC.	2021-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                64.1427(14)
_cell_angle_beta                 64.8810(14)
_cell_angle_gamma                62.8442(14)
_cell_formula_units_Z            6
_cell_length_a                   17.8696(18)
_cell_length_b                   19.2980(19)
_cell_length_c                   19.609(2)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.16
_cell_measurement_theta_min      2.28
_cell_volume                     5195.3(9)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART 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  0.0294
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            77586
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.194
_diffrn_reflns_theta_min         1.203
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.983
_exptl_absorpt_correction_T_max  0.2638
_exptl_absorpt_correction_T_min  0.2010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3102
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.152
_refine_diff_density_max         4.569
_refine_diff_density_min         -1.978
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1388
_refine_ls_number_reflns         28023
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+20.1987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22896
_reflns_number_total             28023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05904a2.cif
_cod_data_source_block           src23
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7129459
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.352
_shelx_estimated_absorpt_t_max   0.518
_exptl_absorpt_special_details
; 
Reflections not merged 
77601 Corrected reflections written to file src23s.hkl 
Estimated minimum and maximum transmission:  0.2010  0.2638 
The ratio (0.7619) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  1.0000 
Lambda/2 correction factor = 0.00150 
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_shelx_res_checksum              6678