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_7707958
_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 Pr2'
_chemical_formula_sum            'C72 H96 B12 P6 Pr2'
_chemical_formula_weight         1558.84
_chemical_name_common            Pr(Ph-PDB)3
_chemical_name_systematic        Pr2(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             2019-09-02
_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                 107.636(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.239(4)
_cell_length_b                   9.6296(10)
_cell_length_c                   23.924(2)
_cell_measurement_reflns_used    8981
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.2955
_cell_volume                     8175.9(14)
_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 0.994
_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  0.1012
_diffrn_reflns_av_unetI/netI     0.0883
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_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            108446
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.431
_diffrn_reflns_theta_min         1.703
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0680 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.9123.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       lath-like
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.054
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         16695
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+47.5032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10259
_reflns_number_total             16695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01932e2.cif
_cod_data_source_block           dal1930
_cod_depositor_comments
'Adding full bibliography for 7707952--7707958.cif.'
_cod_database_code               7707958
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H) groups
2. Restrained distances
 C11-C12 = C12-C13 = C13-C14 = C14-C15 = C15-C16 = C16-C11
 1.39 with sigma of 0.01
 C11A-C12A = C12A-C13A = C13A-C14A = C14A-C15A = C15A-C16A = C16A-C11A
 1.39 with sigma of 0.01
 C21-C22 = C22-C23 = C23-C24 = C24-C25 = C25-C26 = C26-C21
 1.39 with sigma of 0.01
 C21A-C22A = C22A-C23A = C23A-C24A = C24A-C25A = C25A-C26A = C26A-C21A
 1.39 with sigma of 0.01
 C31-C32 = C32-C33 = C33-C34 = C34-C35 = C35-C36 = C36-C31
 1.39 with sigma of 0.01
 C31A-C32A = C32A-C33A = C33A-C34A = C34A-C35A = C35A-C36A = C36A-C31A
 1.39 with sigma of 0.01
 C41-C42 = C42-C43 = C43-C44 = C44-C45 = C45-C46 = C46-C41
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(C15A) =
Uanis(C16A) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) =
Uanis(C16)
Uanis(C11A) = Uanis(P1) = Uanis(P1) = Uanis(C11A) = Uanis(C11) = Uanis(P1) =
Uanis(P1) = Uanis(C11)
Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26) =
Uanis(C21A) = Uanis(C22A) = Uanis(C23A) = Uanis(C24A) = Uanis(C25A) =
Uanis(C26A)
Uanis(C21A) = Uanis(P1) = Uanis(P1) = Uanis(C21A) = Uanis(C21) = Uanis(P1) =
Uanis(P1) = Uanis(C21)
Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) =
Uanis(C31A) = Uanis(C32A) = Uanis(C33A) = Uanis(C34A) = Uanis(C35A) =
Uanis(C36A)
Uanis(C31) = Uanis(P2) = Uanis(P2) = Uanis(C31) = Uanis(C31A) = Uanis(P2) =
Uanis(P2) = Uanis(C31A)
Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46)
4. Others
 Sof(C12A)=Sof(H12D)=Sof(C11A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=1-FVAR(1)
 Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(H16)=FVAR(1)
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=
 Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C21A)=1-FVAR(2)
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=FVAR(2)
 Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=
 Sof(H36A)=Sof(C31A)=Sof(C32A)=Sof(H32A)=1-FVAR(3)
 Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=
 Sof(C31)=Sof(C32)=Sof(H32)=FVAR(3)
5.a Free rotating group:
 C11(C12,C13,C14,C15,C16), C22A(C23A,C24A,C25A,C26A,C21A), C33(C34,C35,C36,C31,
 C32)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C12A(H12D), C13A(H13A),
 C14A(H14A), C15A(H15A), C16A(H16A), C22(H22), C23(H23), C24(H24), C25(H25),
 C26(H26), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C33(H33),
  C34(H34), C35(H35), C36(H36), C32(H32), C33A(H33A), C34A(H34A), C35A(H35A),
 C36A(H36A), C32A(H32A), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76),
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86), C92(H92), C93(H93), C94(H94),
  C95(H95), C96(H96), C102(H102), C103(H103), C104(H104), C105(H105),
 C106(H106), C112(H112), C113(H113), C114(H114), C115(H115), C116(H116),
 C122(H122), C123(H123), C124(H124), C125(H125), C126(H126)
5.c Fitted hexagon refined as free rotating group:
 C33A(C34A,C35A,C36A,C31A,C32A)
5.d Idealised Me refined as rotating group:
 B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), B3(H3A,H3B,H3C), B4(H4A,H4B,H4C), B5(H5A,
 H5B,H5C), B6(H6A,H6B,H6C), B7(H7A,H7B,H7C), B8(H8A,H8B,H8C), B9(H9A,H9B,H9C),
 B10(H10A,H10B,H10C), B11(H11A,H11B,H11C), B12(H12A,H12B,H12C)
;
_shelx_res_checksum              38081
_shelx_hkl_checksum              53527
_olex2_submission_special_instructions 'No special instructions were received'