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_7707956
_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         'C12 H24 B2 I2 O3 P U'
_chemical_formula_sum            'C12 H24 B2 I2 O3 P U'
_chemical_formula_weight         760.73
_chemical_name_common            U(H-PDB)
_chemical_name_systematic        U(BH3Ph2BH3)I2(THF)3
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5213(11)
_cell_length_b                   15.3494(17)
_cell_length_c                   15.8099(18)
_cell_measurement_reflns_used    7113
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.517
_cell_volume                     2310.6(5)
_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 0.966
_diffrn_measurement_device_type  'D8 Ventere Duo'
_diffrn_measurement_method       'Photon 3 Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         2.517
_exptl_absorpt_coefficient_mu    9.770
_exptl_absorpt_correction_T_max  0.4920
_exptl_absorpt_correction_T_min  0.3139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0940 before and 0.0438 after correction.
The Ratio of minimum to maximum transmission is 0.6380.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_description       'rod like'
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.085
_refine_diff_density_max         4.078
_refine_diff_density_min         -3.495
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         2777
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0882P)^2^+44.3811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2079
_reflns_number_total             2777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01932e2.cif
_cod_data_source_block           dal201
_cod_depositor_comments
'Adding full bibliography for 7707952--7707958.cif.'
_cod_database_code               7707956
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.491
_shelx_estimated_absorpt_t_min   0.127
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All B(H,H,H) groups
2. Restrained distances
 P1-H1
 1.3 with sigma of 0.02
 H1-H1_$1
 2.1 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(U1) = Uanis(O1) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) =
Uanis(O1A) = Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A)
4. Others
 Sof(C11)=Sof(C14)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=
 Sof(O1A)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(O1)=Sof(C11A)=
 Sof(C14A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C12(H12A,H12B), C13(H13A,H13B), C12A(H12C,
 H12D), C13A(H13C,H13D)
5.b Idealised Me refined as rotating group:
 B1(H1A,H1B,H1C)
;
_shelx_res_checksum              15235
_shelx_hkl_checksum              22643
_olex2_submission_special_instructions 'No special instructions were received'