Systematic studies of hexanuclear {MIII4LnIII2} complexes (M = Fe, Ga; Ln = Er, Ho): structures, magnetic properties and SMM behavior
Chen, Sihuai; Mereacre, Valeriu; Kostakis, George E.; Anson, Christopher E.; Powell, Annie K.; Inorganic Chemistry Frontiers 4 (2017) 927–; doi:10.1039/C7QI00091J

data_4349687
_publ_section_title
;
 Systematic studies of hexanuclear {MIII4LnIII2} complexes (M = Fe, Ga; Ln
 = Er, Ho): structures, magnetic properties and SMM behavior
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              927
_journal_paper_doi               10.1039/C7QI00091J
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C88 H110 Fe4 Ho2 N4 O26, C2 H3 N'
_chemical_formula_sum            'C90 H113 Fe4 Ho2 N5 O26'
_chemical_formula_weight         2234.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/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
;
2016-09-19 deposited with the CCDC.
2017-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.221(4)
_cell_length_b                   29.282(5)
_cell_length_c                   22.420(5)
_cell_measurement_reflns_used    7996
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.02
_cell_volume                     9504(4)
_computing_cell_refinement       'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_data_collection       'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_data_reduction        'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_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    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      243(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detector, \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58808
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.978
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.315
_exptl_absorpt_correction_T_max  0.551
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             4536
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.273
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00155(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1141
_refine_ls_number_reflns         16957
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0703P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11731
_reflns_number_total             16957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00091j2.cif
_cod_data_source_block           a657ho
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349687
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.543
_shelx_estimated_absorpt_t_max   0.655
_shelx_res_checksum              31206
_shelx_hkl_checksum              52563