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_7118295
_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 Tb3, 4(H2 O), 7(C H4 O)'
_chemical_formula_sum            'C106 H135 Fe6 N6 O50 Tb3'
_chemical_formula_weight         3105.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-12 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.572(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.189(3)
_cell_length_b                   26.117(3)
_cell_length_c                   20.479(2)
_cell_measurement_reflns_used    11004
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.81
_cell_measurement_theta_min      2.25
_cell_volume                     12855(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.912
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30941
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.094
_diffrn_reflns_theta_min         1.972
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.553
_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    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             6256
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         2.875
_refine_diff_density_min         -1.523
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         14288
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0779P)^2^+33.8442P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11040
_reflns_number_total             14288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08887a2.cif
_cod_data_source_block           14eik
_cod_original_cell_volume        12854(2)
_cod_database_code               7118295
_shelx_estimated_absorpt_t_min   0.557
_shelx_estimated_absorpt_t_max   0.852
_shelxl_version_number           2013-2
_shelx_res_checksum              83103
_shelx_hkl_checksum              75692