Ultra-low temperature structure determination of a Mn12 single-molecule magnet and the interplay between lattice solvent and structural disorder
Farrell, Andrew R.; Coome, Jonathan A.; Probert, Michael R.; Goeta, Andrès E.; Howard, Judith A. K.; Lemée-Cailleau, Marie-Hélène; Parsons, Simon; Murrie, Mark; CrystEngComm 15 (2013) 3423–; doi:10.1039/c3ce00042g

data_7210675
_publ_section_title
;
 Ultra-low temperature structure determination of a Mn12 single-molecule
 magnet and the interplay between lattice solvent and structural disorder
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              3423
_journal_paper_doi               10.1039/c3ce00042g
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_compound_source        AF37A
_chemical_formula_moiety         '[Mn12O12(OAc)16(H2O)4].4H2O'
_chemical_formula_sum            'C32 H64 Mn12 O52'
_chemical_formula_weight         1939.96
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   'difmap and calculated'
_atom_sites_solution_primary     'charge flipping'
_audit_creation_date             12-08-23
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.235(4)
_cell_length_b                   17.235(4)
_cell_length_c                   12.038(3)
_cell_measurement_reflns_used    1253
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      1.000
_cell_volume                     3575.8(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.019
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2469
_diffrn_reflns_theta_full        25.034
_diffrn_reflns_theta_max         25.034
_diffrn_reflns_theta_min         2.363
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.144
_exptl_absorpt_correction_T_max  1.044
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1944
_exptl_crystal_recrystallization_method
;
Crystals of Mn12-acetate were heated to 130 C under an N2 atmosphere
for two hours.
;
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details 'Flack (1983), 839 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1297
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         2385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.0003172
_refine_ls_shift/su_mean         0.0000409
_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:
3.34 -2.65 0.900
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0372
_refine_ls_wR_factor_gt          0.0329
_refine_ls_wR_factor_ref         0.0332
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                2351
_reflns_number_total             2466
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.70
_oxford_diffrn_Wilson_scale      1.83
_oxford_refine_ls_r_factor_ref   0.0445
_oxford_refine_ls_scale          0.8034(11)
_oxford_reflns_number_all        2436
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'Mn12_H2O in I-4'
_cod_data_source_file            c3ce00042g.txt
_cod_data_source_block           Mn12_H2O
_cod_original_cell_volume        3576.0(14)
_cod_original_sg_symbol_H-M      'I -4 '
_cod_database_code               7210675
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, MN(1,U'S) UNTIL O(7)
CONT ENANTIO
CONT C(31,U[ISO]) UNTIL C(42)
CONT O(8,U'S) UNTIL O(13)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S)
RIDE C ( 41,X'S) H ( 411,X'S) H ( 412,X'S) H ( 413,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S)
RIDE O ( 12,X'S) H ( 121,X'S) H ( 122,X'S)
RIDE O ( 13,X'S) H ( 131,X'S) H ( 132,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;