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_7705522
_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 O2 Tb, C4 H8 O'
_chemical_formula_sum            'C51 H45 F12 N6 O3 Tb'
_chemical_formula_weight         1176.85
_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   mixed
_audit_creation_date             2018-08-08
_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                85.87(3)
_cell_angle_beta                 75.52(3)
_cell_angle_gamma                69.45(3)
_cell_formula_units_Z            4
_cell_length_a                   13.510(3)
_cell_length_b                   18.030(4)
_cell_length_c                   22.570(5)
_cell_measurement_reflns_used    15932
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     4984(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    'SHELXS-97 (Sheldrick, 1997)'
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0360
_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            104447
_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         26.372
_diffrn_reflns_theta_min         1.512
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.860
_exptl_transmission_factor_min   0.762
_refine_diff_density_max         1.993
_refine_diff_density_min         -2.442
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1359
_refine_ls_number_reflns         19931
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+9.4240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15922
_reflns_number_total             19931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03044a2.cif
_cod_data_source_block           m_a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7705503--7705523.cif.'
_cod_original_cell_volume        4983(2)
_cod_database_code               7705522
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.772
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 F19, C81
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C101, C100
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C101 \\sim C100: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001
4. Others
 Fixed Sof: O6(0.5) C54(0.5) H54A(0.5) H54B(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 O3(0.5) C48(0.5) H48B(0.5) H48A(0.5) C49(0.5) H49A(0.5) H49B(0.5) C50(0.5)
 H50A(0.5) H50B(0.5) C53(0.5) H53A(0.5) H53B(0.5) C52(0.5) H52A(0.5) H52B(0.5)
 C1AA(0.5) H1AA(0.5) H1AB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C99(H99A,H99B), C45(H45A,H45B), C40(H40A,H40B), C98(H98A,
 H98B), C44(H44A,H44B), C95(H95A,H95B), C43(H43A,H43B), C42(H42A,H42B),
 C97(H97A,H97B), C41(H41A,H41B), C96(H96A,H96B), C100(H10A,H10B), C102(H10C,
 H10D), C46(H46A,H46B), C105(H10G,H10H), C104(H10I,H10J), C106(H10K,H10L),
 C101(H10E,H10F), C107(H10M,H10N), C54(H54A,H54B), C55(H55A,H55B), C48(H48B,
 H48A), C49(H49A,H49B), C50(H50A,H50B), C53(H53A,H53B), C52(H52A,H52B),
 C1AA(H1AA,H1AB)
5.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C62(H62), C20(H20), C7(H7), C88(H88), C93(H93), C17(H17), C25(H25),
 C65(H65), C92(H92), C57(H57), C71(H71), C91(H91), C75(H75), C58(H58), C12(H12),
  C23(H23), C70(H70), C66(H66), C36(H36), C72(H72), C37(H37), C10(H10),
 C67(H67), C11(H11), C15(H15), C38(H38), C16(H16), C59(H59), C86(H86), C30(H30),
  C28(H28), C29(H29), C85(H85), C84(H84), C2(H2), C4(H4), C80(H80), C0AA(H0AA),
 C79(H79), C78(H78)
;
_olex2_submission_special_instructions 'No special instructions were received'