Exploring the effect of the Ln(III)/Ln(II) redox potential on C-F activation and on oxidation of some lanthanoid organoamides.
Deacon, Glen B.; Junk, Peter C.; Kelly, Rory P.; Wang, Jun; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1422–1435; doi:10.1039/c5dt04239a

data_7037601
_publ_section_title
;
 Exploring the effect of the Ln(III)/Ln(II) redox potential on C-F
 activation and on oxidation of some lanthanoid organoamides.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1422
_journal_page_last               1435
_journal_paper_doi               10.1039/c5dt04239a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C60 H66 F27 N12 Sm3, 1.5(C7 H8)'
_chemical_formula_sum            'C70.5 H78 F27 N12 Sm3'
_chemical_formula_weight         2057.49
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-28 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   22.323(3)
_cell_length_b                   22.323(3)
_cell_length_c                   53.058(11)
_cell_measurement_reflns_used    125838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.787
_cell_measurement_theta_min      1.123
_cell_volume                     22897(6)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     0.71196
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            118269
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.499
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.123
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    2.394
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             12168
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_refine_diff_density_max         2.710
_refine_diff_density_min         -2.977
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11581
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0763P)^2^+226.3409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8912
_reflns_number_total             11581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04239a1.cif
_cod_data_source_block           added_by_encifer
_cod_depositor_comments
'Adding full bibliography for 7037593--7037603.cif.'
_cod_original_cell_volume        22897(8)
_cod_original_formula_sum        'C70.50 H78 F27 N12 Sm3'
_cod_database_code               7037601
_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 C(H,H,H) groups
2. Restrained distances
 C42-C43 = C43-C44 = C44-C45 = C45-C46 = C46-C47 = C47-C42
 1.39 with sigma of 0.01
 C41-C42
 1.51 with sigma of 0.01
 C42-C44 = C43-C45 = C44-C46 = C45-C47 = C46-C42 = C47-C43
 2.38 with sigma of 0.02
3. Restrained planarity
 C41, C42, C43, C44, C45, C46, C47
 with sigma of 0.1
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C17(H17A,H17B), C18(H18A,H18B), C27(H27A,H27B),
 C28(H28A,H28B), C37(H37A,H37B), C38(H38A,H38B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C24(H24), C34(H34), C43(H43), C44(H44), C45(H45), C46(H46),
 C47(H47)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'