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_7705519
_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         'C58 H86 F N4 Nd O2'
_chemical_formula_sum            'C58 H86 F N4 Nd O2'
_chemical_formula_weight         1034.54
_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
_audit_creation_date             2019-08-09
_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                90
_cell_angle_beta                 95.019(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5982(2)
_cell_length_b                   22.8059(4)
_cell_length_c                   22.1814(4)
_cell_measurement_reflns_used    30014
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      30.9270
_cell_measurement_theta_min      3.3750
_cell_volume                     5340.72(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -10.00  77.00   0.50   18.00    --    4.17  53.00  53.00  174
  2  \w    -18.00  66.00   0.50   18.00    --   -5.03  57.00 120.00  168
  3  \w    -26.00  12.00   0.50   18.00    --   -5.03 -77.00  30.00   76
  4  \w    -53.00 -27.00   0.50   18.00    --   -5.03 -77.00  30.00   52
  5  \w    -63.00  18.00   0.50   18.00    --    4.17 -53.00 -91.00  162
  6  \w    -18.00   7.00   0.50   18.00    --   -5.03 -99.00 -90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0291215000
_diffrn_orient_matrix_UB_12      -0.0189860000
_diffrn_orient_matrix_UB_13      0.0199961000
_diffrn_orient_matrix_UB_21      0.0482064000
_diffrn_orient_matrix_UB_22      0.0065841000
_diffrn_orient_matrix_UB_23      0.0232357000
_diffrn_orient_matrix_UB_31      -0.0366224000
_diffrn_orient_matrix_UB_32      0.0237292000
_diffrn_orient_matrix_UB_33      0.0095510000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61941
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.807
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       block
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.433
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         13754
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+6.8153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11146
_reflns_number_total             13754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03044a2.cif
_cod_data_source_block           gzf190801
_cod_depositor_comments
'Adding full bibliography for 7705503--7705523.cif.'
_cod_database_code               7705519
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         NdCHNFO
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.822
_diffrn_oxdiff_digest_frames
;
015c655489d3d5e37606cd6b0b89437c1f00025337d
;
_diffrn_oxdiff_digest_hkl
;
019daabf7cdc536293dc9757cdccc80ea972c1
;
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C56, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57A, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C56 \\sim C55: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001
C57A \\sim C57: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001
4. Others
 Fixed Sof: H56A(0.75) H56B(0.75) H56C(0.25) H56D(0.25) C58(0.75) H58A(0.75)
 H58B(0.75) C58A(0.25) H58C(0.25) H58D(0.25) C57(0.75) H57A(0.75) H57B(0.75)
 C57A(0.25) H57C(0.25) H57D(0.25)
5.a Ternary CH refined with riding coordinates:
 C28(H28), C41(H41), C23(H23), C35(H35), C3(H3), C16(H16), C48(H48), C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C54(H54A,H54B), C52(H52A,H52B), C55(H55A,H55B), C53(H53A,
 H53B), C56(H56A,H56B), C56(H56C,H56D), C58(H58A,H58B), C58A(H58C,H58D),
 C57(H57A,H57B), C57A(H57C,H57D)
5.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C13(H13), C19(H19), C5(H5), C7(H7), C30(H30), C6(H6), C21(H21),
 C32(H32), C20(H20), C46(H46), C45(H45), C44(H44), C31(H31)
5.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C25(H25A,H25B,H25C), C37(H37A,
 H37B,H37C), C50(H50A,H50B,H50C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C),
 C2(H2A,H2B,H2C), C49(H49A,H49B,H49C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
  C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.896