A Record Anisotropy Barrier for a Single-Molecule Magnet
Constantinos J. Milios; Alina Vinslava; Wolfgang Wernsdorfer; Stephen Moggach; Simon Parsons; Spyros P. Perlepes; George Christou; Euan K. Brechin; Journal of the American Chemical Society 129 (2007) 2754–2755; doi:10.1021/ja068961m

data_4109156
_publ_contact_author_name        'Stephen A. Moggach'
_publ_section_title
;
 A Record Anisotropy Barrier for a Single-Molecule Magnet
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2754
_journal_page_last               2755
_journal_paper_doi               10.1021/ja068961m
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C42 H54 Mn3 N3 O12'
_chemical_formula_sum            'C42 H54 Mn3 N3 O12'
_chemical_formula_weight         957.69
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-10-25
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 107.5490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9120(2)
_cell_length_b                   23.5530(4)
_cell_length_c                   15.1900(3)
_cell_measurement_reflns_used    7992
_cell_measurement_temperature    150
_cell_measurement_theta_max      50
_cell_measurement_theta_min      4
_cell_volume                     4404.53(14)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65857
_diffrn_reflns_theta_full        28.008
_diffrn_reflns_theta_max         29.795
_diffrn_reflns_theta_min         1.651
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.56
_refine_diff_density_min         -1.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         11723
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.007955
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 59.0 94.5 57.6 25.3 5.54 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1555
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1555
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6207
_reflns_number_total             11723
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.24015(17)
_oxford_structure_analysis_title eb6142
_cod_data_source_file            ja068961msi20061214_121540.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4109156