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_7705507
_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         'C70 H90 N8 O4 Yb2'
_chemical_formula_sum            'C70 H90 N8 O4 Yb2'
_chemical_formula_weight         1453.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-08-21
_audit_creation_method
;
Olex2 1.3
(compiled Sep 10 2019 10:52:38 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-08-21 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.37(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.250(3)
_cell_length_b                   15.840(3)
_cell_length_c                   17.389(4)
_cell_measurement_reflns_used    289
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     3319.0(13)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 n/a (Burla et al.,  2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.0879
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45312
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.558
_refine_diff_density_min         -1.656
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6495
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0625P)^2^+4.8021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5210
_reflns_number_total             6495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03044a2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7705503--7705523.cif.'
_cod_original_cell_volume        3319.1(12)
_cod_database_code               7705507
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.763
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Yb1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, Yb1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Yb1 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(O1) \\sim Ueq, Uanis(Yb1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 N4, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Yb1, O2, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1(0.4) O1A(0.6)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C23(H23), C2(H2), C9(H9)
6.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C19(H19), C21(H21), C20(H20), C26(H26), C6(H6), C5(H5),
 C27(H27), C30(H30), C35(H35), C31(H31), C28(H28), C29(H29), C34(H34), C33(H33),
  C32(H32)
6.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C11(H11A,H11B,
 H11C), C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              39351
_olex2_submission_special_instructions 'No special instructions were received'