Predictable self-assembled [2 ? 2] Ln(III)4 square grids (Ln = Dy,Tb)-SMM behaviour in a new lanthanide cluster motif
Muhammad Usman Anwar; Laurence Kenneth Thompson; Louise Nicole Dawe; Fatemah Habib; Muralee Murugesu; Chem.Commun. 48 (2012) 4576–; doi:10.1039/c2cc17546k

data_7107620
_publ_section_title
;
 Predictable self-assembled [2 ? 2] Ln(III)4 square grids (Ln = Dy,Tb)-SMM
 behaviour in a new lanthanide cluster motif
;
_journal_name_full               Chem.Commun.
_journal_page_first              4576
_journal_paper_doi               10.1039/c2cc17546k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C60 H58 Dy4 N36 O5, 25(H2 O)'
_chemical_formula_sum            'C60 H108 Dy4 N36 O30'
_chemical_formula_weight         2463.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                84.31(3)
_cell_angle_beta                 86.78(2)
_cell_angle_gamma                71.967(18)
_cell_formula_units_Z            4
_cell_length_a                   19.806(9)
_cell_length_b                   20.037(9)
_cell_length_c                   27.326(15)
_cell_measurement_reflns_used    27149
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      29.8
_cell_measurement_theta_min      1.5
_cell_volume                     10257(9)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-97: Acta Cryst.2008, A64, 112-122'
_computing_structure_solution    'SHELXS-97: Acta Cryst.2008, A64, 112-122'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0948
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40060
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    2.965
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, Private Communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
The Platon SQUEEZE procedure was applied to recover 1014 electrons per
unit cell in one void (total volume 4097 ^A^3); that is 253.5 electrons
per formula unit. Lattice solvent water molecules
(18 electrons/H2O with V(liq) ~29.92^A^3/H2O) were present, and the
electrons recovered by SQUEEZE have been assigned as 25 water
molecules per formula unit. These water molecules have
been included in the formula for the calculation of intensive
properties.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13.
;
_refine_diff_density_max         7.672
_refine_diff_density_min         -3.938
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1907
_refine_ls_number_reflns         40060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.1146
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3069
_refine_ls_wR_factor_ref         0.3419
_reflns_number_gt                24602
_reflns_number_total             40060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc17546k.txt
_cod_data_source_block           2
_cod_database_code               7107620