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_7707957
_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 Nd2 P6'
_chemical_formula_sum            'C72 H96 B12 Nd2 P6'
_chemical_formula_weight         1565.50
_chemical_name_systematic        Nd2(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             2019-08-31
_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                 109.675(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.826(3)
_cell_length_b                   9.6646(17)
_cell_length_c                   23.904(4)
_cell_measurement_reflns_used    3132
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.81
_cell_measurement_theta_min      2.293
_cell_volume                     4095.3(12)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.1449
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45311
_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         26.313
_diffrn_reflns_theta_min         2.293
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0705 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.8683.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.775
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.141
_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     324
_refine_ls_number_reflns         8303
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0647P)^2^+13.5750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4614
_reflns_number_total             8303
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01932e2.cif
_cod_data_source_block           dal1923
_cod_depositor_comments
'Adding full bibliography for 7707952--7707958.cif.'
_cod_database_code               7707957
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.669
_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
 C51-C52 = C52-C53 = C53-C54 = C54-C55 = C55-C56 = C56-C51
 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-C1 = C1-C35A = C35A-C36A = C36A-C31A
 1.39 with sigma of 0.01
 C61-C62 = C62-C63 = C63-C64 = C64-C65 = C65-C66 = C66-C61
 1.39 with sigma of 0.01
 C61A-C62A = C62A-C63A = C63A-C64A = C64A-C65A = C65A-C66A = C66A-C61A
 1.39 with sigma of 0.01
 C11-C12 \\sim C12-C13 \\sim C13-C14 \\sim C14-C15 \\sim C15-C16 \\sim C16-C11
 with sigma of 0.02
 C11A-C12A \\sim C12A-C13A \\sim C13A-C14A \\sim C14A-C15A \\sim C15A-C16A
\\sim C16A-C11A
 with sigma of 0.02
 C21-C22 \\sim C22-C23 \\sim C23-C24 \\sim C24-C25 \\sim C25-C26 \\sim C26-C21
 with sigma of 0.02
 C21A-C22A \\sim C22A-C23A \\sim C23A-C24A \\sim C24A-C25A \\sim C25A-C26A
\\sim C26A-C21A
 with sigma of 0.02
 C31-C32 \\sim C32-C33 \\sim C33-C34 \\sim C34-C35 \\sim C35-C36 \\sim C36-C31
 with sigma of 0.02
 P2-C31 \\sim C31-P2
 with sigma of 0.02
 P2-C31A \\sim C31A-P2
 with sigma of 0.02
 C31A-C32A \\sim C32A-C33A \\sim C33A-C1 \\sim C1-C35A \\sim C35A-C36A \\sim
C36A-C31A
 with sigma of 0.02
 C41-C42 \\sim C42-C43 \\sim C43-C44 \\sim C44-C45 \\sim C45-C46 \\sim C46-C41
 with sigma of 0.02
 C51-C52 \\sim C52-C53 \\sim C53-C54 \\sim C54-C55 \\sim C55-C56 \\sim C56-C51
 with sigma of 0.02
 C51A-C52A \\sim C52A-C53A \\sim C53A-C54A \\sim C54A-C55A \\sim C55A-C56A
\\sim C56A-C51A
 with sigma of 0.02
 P3-C51 \\sim C51-P3
 with sigma of 0.02
 P3-C51A \\sim C51A-P3
 with sigma of 0.02
 C61-C62 \\sim C62-C63 \\sim C63-C64 \\sim C64-C65 \\sim C65-C66 \\sim C66-C61
 with sigma of 0.02
 C61A-C62A \\sim C62A-C63A \\sim C63A-C64A \\sim C64A-C65A \\sim C65A-C66A
\\sim C66A-C61A
 with sigma of 0.02
 P3-C61 \\sim C61-P3
 with sigma of 0.02
 P3-C61A \\sim C61A-P3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) =
Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(C15A) =
Uanis(C16A)
Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46)
Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56)
Uanis(C61A) = Uanis(C62A) = Uanis(C63A) = Uanis(C64A) = Uanis(C65A) =
Uanis(C66A)
Uanis(C31) = Uanis(C36) = Uanis(C35) = Uanis(C1) = Uanis(C34) = Uanis(C33A) =
Uanis(C33) = Uanis(C32A) = Uanis(C32) = Uanis(C31A) = Uanis(C36A) = Uanis(C35A)
Uanis(C31) = Uanis(C31A) = Uanis(C36) = Uanis(C36A) = Uanis(C32A) = Uanis(C32)
= Uanis(C33) = Uanis(C33A) = Uanis(C34) = Uanis(C1) = Uanis(C35A) = Uanis(C35)
Uanis(C21) = Uanis(C21A) = Uanis(C26A) = Uanis(C26) = Uanis(C22A) = Uanis(C25)
= Uanis(C23A) = Uanis(C24) = Uanis(C23) = Uanis(C24A) = Uanis(C25A) = Uanis(C22)
Uanis(C61A) = Uanis(C61) = Uanis(C62A) = Uanis(C62) = Uanis(C66A) = Uanis(C63)
= Uanis(C65A) = Uanis(C64A) = Uanis(C63A) = Uanis(C64) = Uanis(C65) = Uanis(C66)
Uanis(C51) = Uanis(C52) = Uanis(C56A) = Uanis(C56) = Uanis(C55A) = Uanis(C55) =
Uanis(C54) = Uanis(C54A) = Uanis(C53A) = Uanis(C52A) = Uanis(C53)
Uanis(C51A) = Uanis(C51) = Uanis(C52) = Uanis(C56A) = Uanis(C53) = Uanis(C55A)
= Uanis(C54A) = Uanis(C54) = Uanis(C55) = Uanis(C53A) = Uanis(C52A) = Uanis(C56)
4. Others
 Sof(C11A)=Sof(C12A)=Sof(H12A)=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(C26A)=Sof(H26A)=Sof(C22A)=Sof(H22A)=Sof(C25A)=Sof(H25A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(H24A)=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(C31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C1)=Sof(H1)=Sof(C35A)=
 Sof(H35A)=Sof(C36A)=Sof(H36A)=1-FVAR(3)
 Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36)=FVAR(3)
 Sof(C53A)=Sof(H53A)=Sof(C52A)=Sof(H52A)=Sof(C51A)=Sof(C56A)=Sof(H56A)=
 Sof(C55A)=Sof(H55A)=Sof(C54A)=Sof(H54A)=1-FVAR(4)
 Sof(C51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=
 Sof(H55)=Sof(C56)=Sof(H56)=FVAR(4)
 Sof(C61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=Sof(H64A)=
 Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=1-FVAR(5)
 Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=Sof(C65)=
 Sof(H65)=Sof(C66)=Sof(H66)=FVAR(5)
5.a Free rotating group:
 C53A(C52A,C51A,C56A,C55A,C54A)
5.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C46(H46), C45(H45), C44(H44), C42(H42), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A),
 C16A(H16A), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C26A(H26A),
 C22A(H22A), C25A(H25A), C23A(H23A), C24A(H24A), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C32A(H32A), C33A(H33A), C1(H1), C35A(H35A), C36A(H36A),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C53A(H53A), C52A(H52A),
 C56A(H56A), C55A(H55A), C54A(H54A), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A), C66A(H66A)
5.c Idealised Me refined as rotating group:
 B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), B3(H3A,H3B,H3C), B4(H4A,H4B,H4C), B6(H6A,
 H6B,H6C), B5(H5A,H5B,H5C)
;
_shelx_res_checksum              15459
_shelx_hkl_checksum              5474
_olex2_submission_special_instructions 'No special instructions were received'