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_7037603
_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         'C72 H90 Eu4 F26 N12 O2, C7 H8'
_chemical_formula_sum            'C79 H98 Eu4 F26 N12 O2'
_chemical_formula_weight         2349.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-27
_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                90.19(3)
_cell_angle_beta                 91.45(3)
_cell_angle_gamma                95.12(3)
_cell_formula_units_Z            1
_cell_length_a                   11.610(2)
_cell_length_b                   12.902(3)
_cell_length_c                   15.759(3)
_cell_measurement_reflns_used    55920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.244
_cell_measurement_theta_min      3.026
_cell_volume                     2350.4(8)
_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 0.935
_diffrn_measured_fraction_theta_max 0.935
_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     0.7108
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55920
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'Australian Synchrotron'
_exptl_absorpt_coefficient_mu    2.732
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rect. prism'
_exptl_crystal_F_000             1158
_platon_squeeze_details
;
 Spek, A.L. (1990), Acta Cryst. A46, C-34
;
_refine_diff_density_max         2.466
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         7745
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0695P)^2^+3.1899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7111
_reflns_number_total             7745
_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_database_code               7037603
_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
 C101-C102 = C102-C103 = C103-C104 = C104-C105 = C105-C106 = C106-C101
 1.38 with sigma of 0.02
 C100-C101
 1.55 with sigma of 0.02
 C100-C102 = C101-C103 = C102-C104 = C103-C105 = C104-C106 = C105-C101
 2.38 with sigma of 0.04
 C100-C102 \\sim C100-C106
 with sigma of 0.02
3. Restrained planarity
 C100, C101, C102, C103, C104, C105, C106
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106: within
1.7A with sigma of 0.007 and sigma for terminal atoms of 0.001
5. Others
 Fixed Sof: C104(0.5) H104(0.5) C102(0.5) H102(0.5) C103(0.5) H103(0.5)
 C100(0.5) H10D(0.5) H10E(0.5) H10F(0.5) C105(0.5) H105(0.5) C106(0.5)
 H106(0.5) C101(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C35(H35A,H35B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C16(H16), C28(H28), C104(H104), C102(H102), C103(H103), C105(H105),
 C106(H106)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C100(H10D,H10E,H10F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'