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_7118301
_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 Y3, 2(H2 O), 9(C H4 O)'
_chemical_formula_sum            'C108 H139 Fe6 N6 O50 Y3'
_chemical_formula_weight         2923.07
_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   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                90
_cell_angle_beta                 125.552(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.172(4)
_cell_length_b                   25.835(3)
_cell_length_c                   20.884(3)
_cell_measurement_reflns_used    8510
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      1.58
_cell_volume                     12805(3)
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector, \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1258
_diffrn_reflns_av_unetI/netI     0.1287
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24944
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        21.965
_diffrn_reflns_theta_max         21.965
_diffrn_reflns_theta_min         2.116
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             6008
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0946P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4379
_reflns_number_total             7807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc08887a2.cif
_cod_data_source_block           ik1798_sq
_cod_database_code               7118301
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.692
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              59339
_shelx_hkl_checksum              23759
_shelx_fab_checksum              5851