Isolation of uranium(iii) primary phosphido complexes
Perales, Diana; Bhowmick, Rina; Zeller, Matthias; Miro, Pere; Vlaisavljevich, Bess; Bart, Suzanne C.; Chemical Communications  (2022) –; doi:10.1039/D2CC02207A

data_7130511
_publ_section_title
;
 Isolation of uranium(iii) primary phosphido complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02207A
_journal_year                    2022
_chemical_formula_moiety         'C39 H55 B2 N12 P U'
_chemical_formula_sum            'C39 H55 B2 N12 P U'
_chemical_formula_weight         982.57
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-28 deposited with the CCDC.	2022-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                78.759(5)
_cell_angle_beta                 75.724(4)
_cell_angle_gamma                86.939(5)
_cell_formula_units_Z            2
_cell_length_a                   10.9713(8)
_cell_length_b                   11.9909(11)
_cell_length_c                   17.0052(12)
_cell_measurement_reflns_used    6708
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.0839
_cell_measurement_theta_min      3.7579
_cell_volume                     2126.4(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_collection       'Apex3 v2019.11-0 (Bruker, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015a, 2018), 
SHELXLE Rev1117 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonIII_C14 charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27587
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.067
_diffrn_reflns_theta_min         2.730
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    11.435
_exptl_absorpt_correction_T_max  0.1435
_exptl_absorpt_correction_T_min  0.0341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         3.246
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         8734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1059P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6047
_reflns_number_total             8734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02207a3.cif
_cod_data_source_block           dp5167_0m
_cod_database_code               7130511
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.279
_shelx_estimated_absorpt_t_max   0.725
_shelx_res_checksum              9194
_shelx_hkl_checksum              28308