Widely contrasting outcomes from the use of tris(pentafluorophenyl)bismuth or pentafluorophenylsilver as oxidants in the reactions of lanthanoid metals with <i>N</i>,<i>N</i>'-diarylformamidines.
Guo, Zhifang; Blair, Victoria L.; Deacon, Glen B.; Junk, Peter C.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13588–13600; doi:10.1039/d0dt03044a

data_7705520
_publ_section_title
;
 Widely contrasting outcomes from the use of
 tris(pentafluorophenyl)bismuth or pentafluorophenylsilver as oxidants in
 the reactions of lanthanoid metals with
 <i>N</i>,<i>N</i>'-diarylformamidines.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13588
_journal_page_last               13600
_journal_paper_doi               10.1039/d0dt03044a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C47 H37 F12 N6 Nd O2, C4 H8 O'
_chemical_formula_sum            'C51 H45 F12 N6 Nd O3'
_chemical_formula_weight         1162.17
_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
_audit_creation_date             2018-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-21 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                85.52(3)
_cell_angle_beta                 75.40(3)
_cell_angle_gamma                69.60(3)
_cell_formula_units_Z            4
_cell_length_a                   13.580(3)
_cell_length_b                   18.100(4)
_cell_length_c                   22.510(5)
_cell_measurement_reflns_used    20050
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     5018(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            104237
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         0.935
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.893
_exptl_transmission_factor_min   0.850
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.970
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.0063(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1434
_refine_ls_number_reflns         20050
_refine_ls_number_restraints     329
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0964P)^2^+7.2897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14142
_reflns_number_total             20050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03044a2.cif
_cod_data_source_block           m_a
_cod_depositor_comments
'Adding full bibliography for 7705503--7705523.cif.'
_cod_database_code               7705520
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C111-C110 = C110-O8
 2.4 with sigma of 0.02
 C108-C111 = O8-C109
 1.5 with sigma of 0.02
 O8-C111
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(C88) \\sim Ueq, Uanis(C83A) \\sim Ueq, Uanis(F22A) \\sim Ueq, Uanis(C88A)
\\sim Ueq, Uanis(C84A) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(C85A) \\sim Ueq,
Uanis(C86A) \\sim Ueq, Uanis(C87A) \\sim Ueq, : with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C107) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C111) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C109) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F22, C83, C84, C85, C86, C87, C88, C83A, C88A, C84A, F21A, C85A, C86A, C87A,
 F22A, F21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C107, C106, C104, C105, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, C110, C109, C108, C111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C83A)=Sof(F22A)=Sof(C88A)=Sof(C84A)=Sof(F21A)=Sof(C85A)=Sof(H85A)=
 Sof(C86A)=Sof(H86A)=Sof(C87A)=Sof(H87A)=1-FVAR(1)
 Sof(F21)=Sof(F22)=Sof(C83)=Sof(C84)=Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86)=
 Sof(C87)=Sof(H87)=Sof(C88)=FVAR(1)
 Fixed Sof: C106(0.5) H10A(0.5) H10B(0.5) C105(0.5) H10C(0.5) H10D(0.5)
 O7(0.5) C104(0.5) H10E(0.5) H10F(0.5) C107(0.5) H10G(0.5) H10H(0.5) C110(0.5)
 H11A(0.5) H11B(0.5) C109(0.5) H10I(0.5) H10J(0.5) O8(0.5) C111(0.5) H11C(0.5)
 H11D(0.5) C108(0.5) H10K(0.5) H10L(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B),
  C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C99(H99A,H99B), C106(H10A,
 H10B), C105(H10C,H10D), C104(H10E,H10F), C107(H10G,H10H), C110(H11A,H11B),
 C109(H10I,H10J), C111(H11C,H11D), C108(H10K,H10L)
6.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C9(H9), C12(H12), C13(H13), C14(H14), C31(H31),
 C32(H32), C33(H33), C22(H22), C25(H25), C26(H26), C27(H27), C44(H44), C45(H45),
  C46(H46), C35(H35), C38(H38), C39(H39), C40(H40), C65(H65), C66(H66),
 C67(H67), C56(H56), C59(H59), C60(H60), C61(H61), C80(H80), C79(H79), C78(H78),
  C69(H69), C72(H72), C73(H73), C74(H74), C93(H93), C92(H92), C91(H91),
 C82(H82), C85(H85), C86(H86), C87(H87), C85A(H85A), C86A(H86A), C87A(H87A)
;
_shelx_res_checksum              12427
_olex2_submission_special_instructions 'No special instructions were received'