Mechanochemical synthesis and structural analysis of trivalent lanthanide and uranium diphenylphosphinodiboranates.
Fetrow, Taylor V.; Daly, Scott R.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11472–11484; doi:10.1039/d1dt01932e

data_7707954
_publ_section_title
;
 Mechanochemical synthesis and structural analysis of trivalent lanthanide
 and uranium diphenylphosphinodiboranates.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11472
_journal_page_last               11484
_journal_paper_doi               10.1039/d1dt01932e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C72 H96 B12 P6 U2'
_chemical_formula_sum            'C72 H96 B12 P6 U2'
_chemical_formula_weight         1753.08
_chemical_name_common            U(Ph-PDB)3_dimer
_chemical_name_systematic        U2(BH3Ph2BH3)6
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-04
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-09 deposited with the CCDC.	2021-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.622(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8498(19)
_cell_length_b                   9.6187(10)
_cell_length_c                   23.960(2)
_cell_measurement_reflns_used    6131
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.745
_cell_measurement_theta_min      2.3015
_cell_volume                     4091.9(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II'
_diffrn_measurement_method       'CCD Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47507
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.446
_diffrn_reflns_theta_min         2.396
_exptl_absorpt_coefficient_mu    4.107
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0648 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.8731.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.662
_refine_diff_density_min         -1.989
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         8365
_refine_ls_number_restraints     625
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0407P)^2^+16.1993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5566
_reflns_number_total             8365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01932e2.cif
_cod_data_source_block           dal1929
_cod_depositor_comments
'Adding full bibliography for 7707952--7707958.cif.'
_cod_database_code               7707954
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.661
_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 B(H,H,H) groups
2. Restrained distances
 P2A-C19A = P2A-C13A = P2-C13
 1.9 with sigma of 0.01
 C31-C32 \\sim C32-C33 \\sim C33-C34 \\sim C34-C35 \\sim C36-C31 \\sim C25-C26
\\sim C26-C27 \\sim C27-C28
 \\sim C28-C29 \\sim C29-C30 \\sim C25-C30 \\sim C25-C26A \\sim C26A-C27A \\sim
C27A-C28 \\sim C28-C29A ~
 C29A-C30A \\sim C25-C30A \\sim C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim
C5-C6 \\sim C1-C6 \\sim C7-C8A
 \\sim C8A-C9A \\sim C9A-C10A \\sim C10A-C11A \\sim C11A-C12A \\sim C7-C12A
\\sim C19-C20 \\sim C20-C21 ~
 C21-C22 \\sim C22-C23 \\sim C23-C24 \\sim C19-C24
 with sigma of 0.02
3. Restrained planarity
 C13, C14, C15, C16, C17, C18
 with sigma of 0.02
 C13A, C14A, C15A, C16A, C17A, C18A
 with sigma of 0.02
 C25, C28, C26, C27, C29, C30
 with sigma of 0.02
 C25, C28, C26A, C27A, C29A, C30A
 with sigma of 0.02
 C7, C8A, C9A, C10A, C11A, C12A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
B3 \\sim B4 \\sim B3A \\sim B4A: within 1.7A with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(B3) = Uanis(B4) = Uanis(B3A) = Uanis(B4A)
Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24)
Uanis(C19A) = Uanis(C20A) = Uanis(C21A) = Uanis(C22A) = Uanis(C23A) =
Uanis(C24A)
Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) =
Uanis(C13A) = Uanis(C14A) = Uanis(C15A) = Uanis(C16A) = Uanis(C17A) =
Uanis(C18A)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6)
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) =
Uanis(C8A) = Uanis(C9A) = Uanis(C10A) = Uanis(C11A) = Uanis(C12A)
5. Others
 Sof(H28A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(H30A)=1-FVAR(1)
 Sof(H28)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C29)=Sof(H29)=Sof(C30)=
 Sof(H30)=FVAR(1)
 Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=1-FVAR(2)
 Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17)=Sof(C18)=Sof(H18)=FVAR(2)
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=
 Sof(C12A)=Sof(H12A)=1-FVAR(3)
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=
 Sof(H12)=FVAR(3)
 Sof(P2A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(B3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(H3AC)=Sof(B4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(4)
 Sof(P2)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(B3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(B4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(4)
6.a :
 C1(C2,C3,C4,C5,C6), C31(C32,C33,C34,C35,C36)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C28(H28), C28(H28A), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30),
 C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C14A(H14A), C15A(H15A),
  C16A(H16A), C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A), C22A(H22A),
 C23A(H23A), C24A(H24A), C26A(H26A), C27A(H27A), C29A(H29A), C30A(H30A)
6.c Idealised Me refined as rotating group:
 B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), B5(H5A,H5B,H5C), B6(H6A,H6B,H6C), B3(H3A,
 H3B,H3C), B4(H4A,H4B,H4C), B3A(H3AA,H3AB,H3AC), B4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              45514
_shelx_hkl_checksum              51295
_olex2_submission_special_instructions 'No special instructions were received'