Mixed-Valent Mn Supertetrahedra and Planar Discs as Enhanced Magnetic Coolers
Maria Manoli; Anna Collins; Simon Parsons; Andrea Candini; Marco Evangelisti; Euan K. Brechin; Journal of the American Chemical Society 130 (2008) 11129–11139; doi:10.1021/ja802829d

data_4108207
_publ_contact_author_address
; 
 School of Chemistry, 
 Joseph Black Building, 
 King's Buildings, 
 West Mains Road, 
 Edinburgh, EH9 3JJ, UK. 
;
_publ_contact_author_email       anna.collins@ed.ac.uk
_publ_contact_author_name        'Anna Collins'
_publ_contact_author_phone       '+44 131 650 4806'
_publ_section_title
;
 Mixed-Valent Mn Supertetrahedra and Planar Discs as Enhanced Magnetic
 Coolers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11129
_journal_page_last               11139
_journal_paper_doi               10.1021/ja802829d
_journal_volume                  130
_journal_year                    2008
_chemical_compound_source        'Maria Manoli, MMD208'
_chemical_formula_moiety
;
C40 H99.80 I2.20 Mn10 N10 O25.80, 5I, 5(C6 H14)
;
_chemical_formula_sum            'C70 H169.8 I7.2 Mn10 N10 O25.8'
_chemical_formula_weight         3027.75
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-08-20
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.8200(3)
_cell_length_b                   15.8200(3)
_cell_length_c                   77.614(3)
_cell_measurement_reflns_used    6778
_cell_measurement_temperature    150
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     16822.2(8)
_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    'Superflip (Palatinus & Chapuis, 2006)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_device_type  Area
_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  0.047
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       109
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11323
_diffrn_reflns_theta_full        29.008
_diffrn_reflns_theta_max         30.534
_diffrn_reflns_theta_min         1.509
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.132
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.79
_exptl_crystal_description       plate
_exptl_crystal_F_000             6850.800
_exptl_crystal_recrystallization_method
;
From n-hexane.
;
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.10
_platon_squeeze_details          ' ?'
_refine_diff_density_max         2.07
_refine_diff_density_min         -1.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0139
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4129
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.1430
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.000829
_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: 
 0.467 0.416 0.192 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1548
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0812
_reflns_limit_h_max              11
_reflns_limit_h_min              -22
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              109
_reflns_limit_l_min              0
_reflns_number_gt                4129
_reflns_number_total             11323
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.22
_oxford_diffrn_Wilson_scale      11956.06
_oxford_refine_ls_r_factor_ref   0.0779
_oxford_refine_ls_scale          0.01255(3)
_oxford_reflns_number_all        11323
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            ja802829d-file001_2.cif
_cod_data_source_block           EB7122
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C70 H169.80 I7.20 Mn10 N10 O25.80'
_cod_database_code               4108207