Synthesis, Structure, and Magnetism of a Family of Heterometallic {Cu2Ln7} and {Cu4Ln12} (Ln = Gd, Tb, and Dy) Complexes: The Gd Analogues Exhibiting a Large Magnetocaloric Effect
Langley, Stuart K.; Moubaraki, Boujemaa; Tomasi, Corrado; Evangelisti, Marco; Brechin, Euan K.; Murray, Keith S.; Inorganic Chemistry  (2014) 141119100121008–; doi:10.1021/ic5023467

data_4341685
_publ_section_title
;
 Synthesis, Structure, and Magnetism of a Family of Heterometallic
 {Cu2Ln7} and {Cu4Ln12} (Ln = Gd, Tb, and Dy) Complexes: The Gd Analogues
 Exhibiting a Large Magnetocaloric Effect
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              141119100121008
_journal_paper_doi               10.1021/ic5023467
_journal_year                    2014
_chemical_formula_sum            'C142 H202 Cl8 Cu4 Dy12 N6 O66'
_chemical_formula_weight         5536.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                64.34(3)
_cell_angle_beta                 63.89(3)
_cell_angle_gamma                86.39(3)
_cell_formula_units_Z            1
_cell_length_a                   17.789(4)
_cell_length_b                   17.868(4)
_cell_length_c                   18.447(4)
_cell_measurement_reflns_used    58565
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.58
_cell_volume                     4686(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'scans in phi'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_radiation_source         '3BM1 dipole'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71078
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_sigmaI/netI    0.0643
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            58565
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    5.355
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.332
_refine_diff_density_min         -1.660
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         15264
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                11273
_reflns_number_total             15264
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5023467_si_006.cif
_cod_data_source_block           c:\x-seed\cu4dy1~1\copy
_cod_original_cell_volume        4686.6(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4341685