Oxidation of europium with ammonium perfluorocarboxylates in liquid ammonia: Pathways to europium(II) carboxylates and hexanuclear europium(III) fluoridocarboxylate complexes
Morsbach, Florian; Klenner, Steffen; Pöttgen, Rainer; Frank, Walter; Dalton Transactions  (2022) –; doi:10.1039/D1DT04204A

data_7709623
_publ_section_title
;
 Oxidation of europium with ammonium perfluorocarboxylates in liquid
 ammonia: Pathways to europium(II) carboxylates and hexanuclear
 europium(III) fluoridocarboxylate complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04204A
_journal_year                    2022
_chemical_formula_moiety         'C54 H6 Eu6 F98 O36, 8(C3 H F5 O2), 2(H4 N )'
_chemical_formula_sum            'C78 H22 Eu6 F138 N2 O52'
_chemical_formula_weight         5352.80
_chemical_name_systematic
;
Bis(ammonium)[dodecakis(\m~2~-pentafluoropropionato)hexakis(pentafluoro-
propionic acid)octa(\m~3~-fluorido)hexaeuropium(III)]-pentafluoropropionic 
acid (1/8)'
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-02 deposited with the CCDC.	2022-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.721(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6214(13)
_cell_length_b                   33.280(2)
_cell_length_c                   26.1987(19)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.29
_cell_volume                     15357.0(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND 4.0 (Crystal Impact, 2012)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            229309
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.504
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.661
_exptl_absorpt_correction_T_max  0.741
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS-2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.315
_exptl_crystal_description       plate
_exptl_crystal_F_000             10160
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.894
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2567
_refine_ls_number_reflns         26839
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0141P)^2^+94.9674P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21715
_reflns_number_total             26839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04204a2.cif
_cod_data_source_block           compd_3
_cod_original_cell_volume        15357.2(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709623
_shelx_estimated_absorpt_t_min   0.427
_shelx_estimated_absorpt_t_max   0.741
_shelx_res_checksum              1224