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_7130509
_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         'C36 H50 B2 N12 P U, 2(C4 H8 O)'
_chemical_formula_sum            'C44 H66 B2 N12 O2 P U'
_chemical_formula_weight         1085.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 92.876(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1859(4)
_cell_length_b                   19.3077(7)
_cell_length_c                   24.7773(10)
_cell_measurement_reflns_used    9282
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.8936
_cell_measurement_theta_min      2.3735
_cell_volume                     4866.7(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Apex3 v2019.1-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015a, 2018), 
SHELXLE Rev1117 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            171405
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.577
_diffrn_reflns_theta_min         2.685
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    3.417
_exptl_absorpt_correction_T_max  0.3812
_exptl_absorpt_correction_T_min  0.3251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D. (2015). J. Appl. Cryst. 48, 3-10.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       plate
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.493
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.00054(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         14904
_refine_ls_number_restraints     320
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0242P)^2^+5.5323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11165
_reflns_number_total             14904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02207a3.cif
_cod_data_source_block           DP_3_92_2_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7130509
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.594
_shelx_estimated_absorpt_t_max   0.935
_shelx_res_checksum              80821
_shelx_hkl_checksum              54810