Nine members of a family of nine-membered cyclic coordination clusters; Fe6Ln3 wheels (Ln = Gd to Lu and Y).
Kühne, Irina A; Mereacre, Valeriu; Anson, Christopher E.; Powell, Annie K.; Chemical communications (Cambridge, England) 52 (2016) 1021–1024; doi:10.1039/c5cc08887a

data_7118299
_publ_section_title
;
 Nine members of a family of nine-membered cyclic coordination clusters;
 Fe6Ln3 wheels (Ln = Gd to Lu and Y).
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1021
_journal_page_last               1024
_journal_paper_doi               10.1039/c5cc08887a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C99 H99 Fe6 N6 O39 Yb3, 13(C H4 O)'
_chemical_formula_sum            'C112 H151 Fe6 N6 O52 Yb3'
_chemical_formula_weight         3267.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-10-12 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                77.520(2)
_cell_angle_beta                 80.860(2)
_cell_angle_gamma                71.740(1)
_cell_formula_units_Z            4
_cell_length_a                   19.6191(15)
_cell_length_b                   22.3573(17)
_cell_length_c                   31.163(3)
_cell_measurement_reflns_used    14378
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.20
_cell_volume                     12612.6(18)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2000)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector, \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.1160
_diffrn_reflns_laue_measured_fraction_full 0.916
_diffrn_reflns_laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47034
_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.087
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    2.963
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       block
_exptl_crystal_F_000             6588
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.130
_refine_diff_density_max         3.774
_refine_diff_density_min         -2.974
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2721
_refine_ls_number_reflns         42242
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0848
_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^)+(0.0857P)^2^+61.8448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.2130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25814
_reflns_number_total             42242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08887a2.cif
_cod_data_source_block           14jik_sq
_cod_original_cell_volume        12612.6(17)
_cod_database_code               7118299
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.415
_shelx_estimated_absorpt_t_max   0.699
_shelx_res_checksum              20314
_shelx_hkl_checksum              82849
_shelx_fab_checksum              91895