SMM Behaviour and Magnetocaloric Effect in Heterometallic 3d-4f Coordination Clusters with High Azide:Metal Ratios
Schmidt, Sebastian; Merkel, Marcel; Kostakis, George E.; Buth, Gernot; Anson, Christopher; Powell, Annie K.; Dalton Trans.  (2017) –; doi:10.1039/C7DT03149A

data_7044505
_publ_section_title
;
 SMM Behaviour and Magnetocaloric Effect in Heterometallic 3d-4f
 Coordination Clusters with High Azide:Metal Ratios
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03149A
_journal_year                    2017
_chemical_formula_moiety
'3(C16 H36 N), C18 H45 Fe3 Gd2 N47 O9, C H2 Cl2, 0.5(C2 H6 O)'
_chemical_formula_sum            'C68 H158 Cl2 Fe3 Gd2 N50 O9.5'
_chemical_formula_weight         2381.38
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-07-03 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                68.741(2)
_cell_angle_beta                 80.570(2)
_cell_angle_gamma                63.397(2)
_cell_formula_units_Z            2
_cell_length_a                   16.989(2)
_cell_length_b                   17.111(2)
_cell_length_c                   22.479(3)
_cell_measurement_reflns_used    9305
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.40
_cell_measurement_theta_min      2.61
_cell_volume                     5445.2(12)
_computing_cell_refinement       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_collection       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'Apex2 (Bruker AXS Inc., 2005)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'Apex2 (Bruker AXS Inc., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector, \w-scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.80039
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            104884
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         30.868
_diffrn_reflns_theta_min         2.204
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    2.338
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS in Apex2 (Bruker AXS Inc., 2005)
;
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.483
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         23862
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0319P)^2^+2.9420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20789
_reflns_number_total             23862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03149a2.cif
_cod_data_source_block           z10teagd_sq
_cod_original_cell_volume        5445.3(13)
_cod_database_code               7044505
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.767
_shelx_estimated_absorpt_t_max   0.955
_shelx_res_checksum              2120
_shelx_fab_checksum              49961