Octanuclear heterometallic FeIII-CeIV pivalate clusters: From a close {Fe4Ce4(μ4-O)4} cage to an open {Fe4Ce4(μ4-O)2(μ3-O)2} core
Baca, Svetlana G.; Amombo Noa, Francoise M.; Öhrström, Lars; Inorganica Chimica Acta 515 (2021) 120038–; doi:10.1016/j.ica.2020.120038

data_1566178
_publ_section_title
;
 Octanuclear heterometallic FeIII-CeIV pivalate clusters: From a close
 {Fe4Ce4(\m4-O)4} cage to an open {Fe4Ce4(\m4-O)2(\m3-O)2} core
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120038
_journal_paper_doi               10.1016/j.ica.2020.120038
_journal_volume                  515
_journal_year                    2021
_chemical_formula_sum            'C49 H104 Ce4 Fe4 N16 O29'
_chemical_formula_weight         2165.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 114.8500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.2664(12)
_cell_length_b                   12.1527(6)
_cell_length_c                   14.2140(7)
_cell_measurement_reflns_used    20302
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.435
_cell_measurement_theta_min      2.677
_cell_volume                     4117.1(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20302
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.435
_diffrn_reflns_theta_min         2.677
_exptl_absorpt_coefficient_mu    2.927
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 3225 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         8397
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0296P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                7590
_reflns_number_total             8397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            SBS182.cif
_cod_data_source_block           SBS182
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1566178
_shelx_shelxl_version_number     2016/6
_exptl_absorpt_special_details
'Absorption corrections were made using the program SADABS (Sheldrick, 1996)'