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_1566177
_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            'C59 H122 Ce4 Fe4 N10 O33'
_chemical_formula_weight         2283.54
_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   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                110.7302(10)
_cell_angle_beta                 98.5246(9)
_cell_angle_gamma                110.7346(10)
_cell_formula_units_Z            1
_cell_length_a                   12.20595(12)
_cell_length_b                   13.30987(16)
_cell_length_c                   15.93445(16)
_cell_measurement_reflns_used    21958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.076
_cell_measurement_theta_min      3.120
_cell_volume                     2150.71(5)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21958
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.060
_diffrn_reflns_theta_max         67.060
_diffrn_reflns_theta_min         3.122
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    21.944
_exptl_absorpt_correction_T_max  0.398
_exptl_absorpt_correction_T_min  0.281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.21a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.205
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         7567
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0461P)^2^+2.8929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6981
_reflns_number_total             7567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            SBS-191.cif
_cod_data_source_block           SBS-191
_cod_original_cell_volume        2150.71(4)
_cod_database_code               1566177
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.317
_shelx_estimated_absorpt_t_max   0.459
_shelx_res_checksum              30219
_shelx_hkl_checksum              45186