Synthesis, structural and magnetic studies of an isostructural family of mixed 3d/4f tetranuclear 'star' clusters.
Chilton, Nicholas F.; Langley, Stuart K.; Moubaraki, Boujemaa; Murray, Keith S.; Chemical communications (Cambridge, England) 46 (2010) 7787–7789; doi:10.1039/c0cc02642e

data_7112890
_publ_section_title
;
 Synthesis, structural and magnetic studies of an isostructural family of
 mixed 3d/4f tetranuclear 'star' clusters.
;
_journal_issue                   41
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7787
_journal_page_last               7789
_journal_paper_doi               10.1039/c0cc02642e
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety
;
C42 H66 Dy Mn3 N2 O18, C15 H21 Mn O6
;
_chemical_formula_sum            'C57 H87 Dy Mn4 N2 O24'
_chemical_formula_weight         1566.55
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             '9 November 2005'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.036(2)
_cell_length_b                   16.036(2)
_cell_length_c                   15.368(3)
_cell_measurement_reflns_used    37598
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      1.60
_cell_volume                     3422.5(9)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'scans in phi'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Australian synchrotron MX1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77501
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37598
_diffrn_reflns_theta_full        26.59
_diffrn_reflns_theta_max         26.59
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    1.871
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0400P)^2^+8.0170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                1821
_reflns_number_total             1851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc02642e.txt
_cod_data_source_block           2_Mn3Dyfinal
_cod_original_sg_symbol_H-M      P-31c
_cod_database_code               7112890