Structure, Magnetism, and Theoretical Study of a Mixed-Valence CoII3CoIII4 Heptanuclear Wheel: Lack of SMM Behavior despite Negative Magnetic Anisotropy
Liviu F. Chibotaru; Liviu Ungur; Christophe Aronica; Hani Elmoll; Guillaume Pilet; Dominique Luneau; Journal of the American Chemical Society 130 (2008) 12445–12455; doi:10.1021/ja8029416

data_4108337
_publ_contact_author_address
; 
Chemical Crystallography Laboratory 
9 Parks Road 
OXFORD OX1 3PD 
;
_publ_contact_author_email       david.watkin@chem.ox.ac.uk
_publ_contact_author_fax         '01865 272 699'
_publ_contact_author_name        'David Watkin'
_publ_contact_author_phone       '01865 270 826'
_publ_section_title
;
 Structure, Magnetism, and Theoretical Study of a Mixed-Valence
 CoII3CoIII4 Heptanuclear Wheel: Lack of SMM Behavior despite Negative
 Magnetic Anisotropy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12445
_journal_page_last               12455
_journal_paper_doi               10.1021/ja8029416
_journal_volume                  130
_journal_year                    2008
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C24 H33 Co3.25 F9 N3 O9 '
_chemical_formula_sum            'C24 H33 Co3.25 F9 N3 O9'
_chemical_formula_weight         884.79
_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             05-02-02
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 101.237(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.409(5)
_cell_length_b                   12.052(5)
_cell_length_c                   20.006(5)
_cell_measurement_reflns_used    3077
_cell_measurement_temperature    293
_cell_measurement_theta_max      20
_cell_measurement_theta_min      1
_cell_volume                     3171.1(19)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_solution
; 
 SIR97 (Altomare et al, 1999) 
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
; 
Nonius Kappa CCD 
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5889
_diffrn_reflns_theta_full        19.626
_diffrn_reflns_theta_max         20.027
_diffrn_reflns_theta_min         2.025
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.911
_exptl_absorpt_correction_T_max  0.00
_exptl_absorpt_correction_T_min  0.00
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' ? '
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       ' ? '
_exptl_crystal_F_000             1755
_exptl_crystal_size_max          0.00
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.2173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         1499
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.010046
_refine_ls_structure_factor_coef F
_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: 
 1.36 1.12 1.27 0.213 0.212 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0692
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0507
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                1499
_reflns_number_total             2954
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ja8029416_si_001.cif
_cod_data_source_block           CRYSTALS_cif
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C24 H33 Co3.25 F9 N3 O9 '
_cod_database_code               4108337