On the usability of salt metathesis reactions for the synthesis of sterically crowded tris-formamidinate Ln(iii) complexes: success and limits. Spontaneous reduction of Eu(iii) to Eu(ii)
Bashirov, Denis A.; Kolybalov, Dmitry S.; Mironova, Olga A.; Sukhikh, Taisiya S.; Konchenko, Sergey N.; New Journal of Chemistry 46 (2022) 11994–12001; doi:10.1039/D2NJ01589G

data_7061550
_publ_section_title
;
 On the usability of salt metathesis reactions for the synthesis of
 sterically crowded tris-formamidinate Ln(iii) complexes: success and
 limits. Spontaneous reduction of Eu(iii) to Eu(ii)
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11994
_journal_page_last               12001
_journal_paper_doi               10.1039/D2NJ01589G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C54 H78 Cl Eu N4 O'
_chemical_formula_sum            'C54 H78 Cl Eu N4 O'
_chemical_formula_weight         986.61
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-11 deposited with the CCDC.	2022-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                84.017(11)
_cell_angle_beta                 78.118(12)
_cell_angle_gamma                80.397(11)
_cell_formula_units_Z            2
_cell_length_a                   11.367(5)
_cell_length_b                   14.758(5)
_cell_length_c                   16.373(6)
_cell_measurement_reflns_used    2454
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.47
_cell_measurement_theta_min      2.67
_cell_volume                     2643.2(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_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  0.1694
_diffrn_reflns_av_unetI/netI     0.2763
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22217
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        24.404
_diffrn_reflns_theta_max         24.403
_diffrn_reflns_theta_min         1.851
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.2118 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.6939. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       prism
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.490
_refine_diff_density_min         -2.026
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         8545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.1985
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0271P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4091
_reflns_number_total             8545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01589g2.cif
_cod_data_source_block           kds103
_cod_depositor_comments
'Adding full bibliography for 7061550--7061554.cif.'
_cod_original_cell_volume        2643.2(17)
_cod_database_code               7061550
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.725
_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.a Ternary CH refined with riding coordinates:
 C117(H117), C120(H120), C129(H129), C132(H132), C217(H217), C220(H220),
 C229(H229), C232(H232)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C21(H21), C113(H113), C114(H114), C115(H115), C125(H125),
 C126(H126), C127(H127), C213(H213), C214(H214), C215(H215), C225(H225),
 C226(H226), C227(H227)
2.d Idealised Me refined as rotating group:
 C118(H11D,H11E,H11F), C119(H11A,H11B,H11C), C121(H12A,H12B,H12C), C122(H12D,
 H12E,H12F), C130(H13D,H13E,H13F), C131(H13A,H13B,H13C), C133(H13J,H13K,H13L),
 C134(H13G,H13H,H13I), C218(H21D,H21E,H21F), C219(H21A,H21B,H21C), C221(H22A,
 H22B,H22C), C222(H22D,H22E,H22F), C230(H23A,H23B,H23C), C231(H23J,H23K,H23L),
 C233(H23D,H23E,H23F), C234(H23G,H23H,H23I)
;
_shelx_res_checksum              74787
_olex2_submission_special_instructions 'No special instructions were received'