Structure and magnetism of a tetrahedral uranium(iii) β-diketiminate complex.
Boreen, Michael A.; Gould, Colin A.; Booth, Corwin H.; Hohloch, Stephan; Arnold, John; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7938–7944; doi:10.1039/d0dt01599g

data_1558142
_publ_section_title
;
 Structure and magnetism of a tetrahedral uranium(iii) \b-diketiminate
 complex.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7938
_journal_page_last               7944
_journal_paper_doi               10.1039/d0dt01599g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C53 H75 N2 O2 U'
_chemical_formula_sum            'C53 H75 N2 O2 U'
_chemical_formula_weight         1010.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-26 deposited with the CCDC.	2020-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.708(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5520(7)
_cell_length_b                   11.9252(4)
_cell_length_c                   21.1347(7)
_cell_measurement_reflns_used    6896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      1.94
_cell_volume                     4778.3(3)
_computing_cell_refinement       'Bruker ApexII suite, 2015'
_computing_data_collection       'Bruker ApexII suite, 2015'
_computing_data_reduction        'Bruker ApexII suite, 2015'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Quasar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            87639
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.403
_diffrn_reflns_theta_min         1.946
_exptl_absorpt_coefficient_mu    3.437
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1018 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.7944.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       plate
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.548
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8786
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0220P)^2^+10.3962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6896
_reflns_number_total             8786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01599g2.cif
_cod_data_source_block           sh051_0m
_cod_depositor_comments
'Adding full bibliography for 1558142--1558143.cif.'
_cod_database_code               1558142
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   'Blessing, 1995'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C27(H27), C48(H48), C51(H51), C39(H39), C36(H36), C12(H12), C15(H15), C24(H24)
3.b Me refined with riding coordinates:
 C28(H28A,H28B,H28C), C40(H40A,H40B,H40C), C52(H52A,H52B,H52C), C50(H50A,H50B,
 H50C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C49(H49A,H49B,H49C), C29(H29A,
 H29B,H29C), C41(H41A,H41B,H41C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C), C53(H53A,H53B,
 H53C), C38(H38A,H38B,H38C)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C34(H34), C46(H46), C2(H2), C44(H44), C21(H21), C22(H22), C45(H45),
 C33(H33), C32(H32), C20(H20), C8(H8), C9(H9)
3.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              70778
_olex2_submission_special_instructions 'No special instructions were received'