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_1558143
_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         'C82 H116 I2 N4 O2 U2, C3 H7'
_chemical_formula_sum            'C85 H123 I2 N4 O2 U2'
_chemical_formula_weight         1962.73
_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
_audit_creation_date             2020-03-19
_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                75.3460(10)
_cell_angle_beta                 80.6320(10)
_cell_angle_gamma                69.9180(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2023(3)
_cell_length_b                   16.5876(6)
_cell_length_c                   22.5734(8)
_cell_measurement_reflns_used    11678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      1.34
_cell_volume                     4137.1(2)
_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      100.02
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Quazar'
_diffrn_measurement_method       'omega phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54187
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.443
_diffrn_reflns_theta_min         1.338
_exptl_absorpt_coefficient_mu    4.702
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1140 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.9234.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       plate
_exptl_crystal_F_000             1934
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.415
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         15102
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0645P)^2^+27.3806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1411
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11678
_reflns_number_total             15102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01599g2.cif
_cod_data_source_block           sh044_0m
_cod_depositor_comments
'Adding full bibliography for 1558142--1558143.cif.'
_cod_database_code               1558143
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C7A)
\\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C8A) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C12(H12), C36A(H36A), C39(H39), C15(H15), C36(H36), C24(H24), C27A(H27A),
 C24A(H24A), C39A(H39A), C27(H27), C12A(H12A), C15A(H15A)
3.b Secondary CH2 refined with riding coordinates:
 C100(H10B,H10C), C101(H10D,H10E)
3.c Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C29A(H29A,H29B,H29C), C41(H41A,H41B,H41C), C28(H28A,H28B,
 H28C), C14(H14A,H14B,H14C), C25A(H25A,H25B,H25C), C38(H38A,H38B,H38C),
 C28A(H28D,H28E,H28F), C17(H17A,H17B,H17C), C41A(H41D,H41E,H41F), C40A(H40A,
 H40B,H40C), C37(H37A,H37B,H37C), C16(H16A,H16B,H16C), C29(H29D,H29E,H29F),
 C26A(H26D,H26E,H26F), C25(H25D,H25E,H25F), C13(H13A,H13B,H13C), C40(H40D,H40E,
 H40F), C14A(H14D,H14E,H14F), C16A(H16D,H16E,H16F), C37A(H37D,H37E,H37F),
 C38A(H38D,H38E,H38F), C13A(H13D,H13E,H13F), C17A(H17D,H17E,H17F), C102(H10F,
 H10G,H10H)
3.d Aromatic/amide H refined with riding coordinates:
 C20(H20), C2(H2), C10(H10), C8(H8), C2A(H2A), C21(H21), C9(H9), C22(H22),
 C34(H34), C21A(H21A), C32(H32), C22A(H22A), C33(H33), C33A(H33A), C10A(H10A),
 C20A(H20A), C32A(H32A), C34A(H34A), C9A(H9A), C8A(H8A)
3.e Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              68932
_olex2_submission_special_instructions 'No special instructions were received'