Metallacryptate Single-Molecule Magnets: Effect of Lower Molecular Symmetry on Blocking Temperature
Curtis M. Zaleski; Ezra C. Depperman; Catherine Dendrinou-Samara; Maria Alexiou; Jeff W. Kampf; Dimitris P. Kessissoglou; Martin L. Kirk; Vincent L. Pecoraro; Journal of the American Chemical Society 127 (2005) 12862–12872; doi:10.1021/ja050951i

data_4111904
_publ_section_title
;
 Metallacryptate Single-Molecule Magnets: Effect of Lower Molecular
 Symmetry on Blocking Temperature
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12862
_journal_page_last               12872
_journal_paper_doi               10.1021/ja050951i
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety
'2(C147 H147 Mn26 N24 O58), 10(C H4 O), 2(Cl O4), 4(H2 O)'
_chemical_formula_sum            'C152 H165 Cl Mn26 N24 O69'
_chemical_formula_weight         4895.97
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           159
_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_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                   20.2656(12)
_cell_length_b                   20.2656(12)
_cell_length_c                   33.203(4)
_cell_measurement_reflns_used    7869
_cell_measurement_temperature    118(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.71
_cell_volume                     11809.4(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      118(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            138757
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.6599
_exptl_absorpt_correction_T_min  0.6011
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             4928
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.073(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         19533
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0703P)^2^+1.9119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                18317
_reflns_number_total             19533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050951isi20050214_023157.cif
_cod_data_source_block           mndpk
_cod_original_cell_volume        11809.4(16)
_cod_database_code               4111904