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_7037596
_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         'C32 H46 Eu F8 N4 O2'
_chemical_formula_sum            'C32 H46 Eu F8 N4 O2'
_chemical_formula_weight         822.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_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                90
_cell_formula_units_Z            8
_cell_length_a                   13.2169(10)
_cell_length_b                   16.1371(11)
_cell_length_c                   33.290(3)
_cell_measurement_temperature    123(1)
_cell_volume                     7100.2(10)
_computing_cell_refinement       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_collection       'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_data_reduction        'Bruker Apex2 v2.0 (Bruker AXS, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1602
_diffrn_reflns_av_unetI/netI     0.1970
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            48952
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         1.402
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.842
_exptl_absorpt_correction_T_max  0.9135
_exptl_absorpt_correction_T_min  0.6819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'bright yellow'
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         16293
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1831
_refine_ls_R_factor_gt           0.0687
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.828
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                7169
_reflns_number_total             16293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt04239a1.cif
_cod_data_source_block           added_by_encifer
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7037593--7037603.cif.
;
_cod_original_cell_volume        7100.1(9)
_cod_database_code               7037596
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.62344 0.37656
2. 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
3. Restrained distances
 C25-C26 = C62-C63
 1.5 with sigma of 0.005
 C30-C31
 1.5 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
N2 \\sim C9 \\sim C10: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
N6 \\sim C41 \\sim C42: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C61 \\sim C62 \\sim C63 \\sim C64: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
N2 \\sim C11 \\sim C2: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C63)
\\sim Ueq, Uanis(C64) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C62) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C33) = Uanis(C34)
Uanis(C43) = Uanis(N6) = Uanis(C54)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B),
 C14(H14A,H14B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B),
  C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C41(H41A,H41B),
 C43(H43A,H43B), C45(H45A,H45B), C46(H46A,H46B), C53(H53A,H53B), C55(H55A,H55B),
  C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,
 H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C18(H18), C38(H38), C50(H50)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C54(H54A,H54B,H54C), C56(H56A,
 H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'