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_4341686
_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            'C68 H118 Cl5 Cu2 Dy7 N4 O45'
_chemical_formula_weight         3153.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.890(6)
_cell_length_b                   11.820(2)
_cell_length_c                   29.220(6)
_cell_measurement_reflns_used    69906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.14
_cell_volume                     11014(4)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            69906
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    5.263
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5948
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.042(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         19071
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+44.5230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                18230
_reflns_number_total             19071
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5023467_si_003.cif
_cod_data_source_block           c:\x-seed\cu2dy7~2\pca21
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               4341686