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_7709622
_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         'C36 H6 Eu6 F62 O36, 2(H4 N)'
_chemical_formula_sum            'C36 H14 Eu6 F62 N2 O36'
_chemical_formula_weight         3140.31
_chemical_name_systematic
;
Bis(ammonium)[dodecakis(\m~2~-trifluoroacetato)hexakis(trifluoroacetic acid)
octa(\m~3~-fluorido)hexaeuropium(III)]
;
_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                 95.521(3)
_cell_angle_gamma                90
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_cell_length_b                   25.5991(8)
_cell_length_c                   27.1945(9)
_cell_measurement_reflns_used    1195
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      2.04
_cell_volume                     8354.0(5)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2009)'
_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    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1348
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50839
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.655
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   SHELXTL
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.497
_exptl_crystal_description       block
_exptl_crystal_F_000             5872
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.110
_refine_diff_density_max         3.976
_refine_diff_density_min         -2.014
_refine_diff_density_rms         0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1420
_refine_ls_number_reflns         14759
_refine_ls_number_restraints     549
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0892
_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^)+(0.1387P)^2^+492.2837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2621
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12450
_reflns_number_total             14759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04204a2.cif
_cod_data_source_block           compd_2
_cod_original_cell_volume        8354.1(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709622
_shelx_estimated_absorpt_t_min   0.517
_shelx_estimated_absorpt_t_max   0.628
_shelx_res_checksum              71936