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_7707955
_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         'C48 H72 B6 Nd O3 P3'
_chemical_formula_sum            'C48 H72 B6 Nd O3 P3'
_chemical_formula_weight         999.06
_chemical_name_common            Pr(Ph-PDB)3(THF)3
_chemical_name_systematic        Nd(BH3Ph2BH3)3(THF)3
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-04
_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                97.233(5)
_cell_angle_beta                 96.868(5)
_cell_angle_gamma                111.125(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5469(19)
_cell_length_b                   14.970(3)
_cell_length_c                   17.592(3)
_cell_measurement_reflns_used    8654
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      2.3015
_cell_measurement_theta_min      23.25
_cell_volume                     2768.9(9)
_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  0.0877
_diffrn_reflns_av_unetI/netI     0.1038
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37473
_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         26.352
_diffrn_reflns_theta_min         2.061
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0728 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.8367.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       lath-like
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.474
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         11206
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0876P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7897
_reflns_number_total             11206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01932e2.cif
_cod_data_source_block           dal1924
_cod_depositor_comments
'Adding full bibliography for 7707952--7707958.cif.'
_cod_database_code               7707955
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.832
_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
 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
 C51-C52 = C52-C53 = C53-C54 = C54-C55 = C55-C56 = C56-C51
 1.39 with sigma of 0.01
 C51A-C52A = C52A-C53A = C53A-C54A = C54A-C55A = C55A-C56A = C56A-C51A
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
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(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56) =
Uanis(C51A) = Uanis(C52A) = Uanis(C53A) = Uanis(C54A) = Uanis(C55A) =
Uanis(C56A)
Uanis(O1) = Uanis(C71) = Uanis(C72) = Uanis(C73) = Uanis(C74) = Uanis(O1A) =
Uanis(C71A) = Uanis(C72A) = Uanis(C73A) = Uanis(C74A)
4. Others
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=
 Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C31A)=1-FVAR(1)
 Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36)=FVAR(1)
 Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=
 Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=1-FVAR(2)
 Sof(C51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=
 Sof(H55)=Sof(C56)=Sof(H56)=FVAR(2)
 Sof(O1A)=Sof(C71A)=Sof(H71C)=Sof(H71D)=Sof(C72A)=Sof(H72C)=Sof(H72D)=
 Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74C)=Sof(H74D)=1-FVAR(3)
 Sof(O1)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=
 Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=FVAR(3)
5.a Free rotating group:
 C32A(C33A,C34A,C35A,C36A,C31A)
5.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C71A(H71C,
 H71D), C72A(H72C,H72D), C73A(H73C,H73D), C74A(H74C,H74D), C81(H81A,H81B),
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C91(H91A,H91B), C92(H92A,H92B),
  C93(H93A,H93B), C94(H94A,H94B)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C42(H42),
 C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55),
  C56(H56), C52A(H52A), C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A),
 C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
5.d Fitted pentagon refined as free rotating group:
 O1A(C71A,C72A,C73A,C74A)
5.e Fitted hexagon refined as free rotating group:
 C51A(C52A,C53A,C54A,C55A,C56A)
5.f 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)
;
_shelx_res_checksum              9497
_shelx_hkl_checksum              12618
_shelx_fab_checksum              58740
_olex2_submission_special_instructions 'No special instructions were received'