Enhancing U(eff) in oxime-bridged [Mn(III)6Ln(III)2] hexagonal prisms.
Rigaux, Guillaume; Inglis, Ross; Morrison, Susan; Prescimone, Alessandro; Cadiou, Cyril; Evangelisti, Marco; Brechin, Euan K.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 4797–4799; doi:10.1039/c1dt10154d

data_7015847
_publ_section_title
;
 Enhancing U(eff) in oxime-bridged [Mn(III)6Ln(III)2] hexagonal prisms.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4797
_journal_page_last               4799
_journal_paper_doi               10.1039/c1dt10154d
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'Ross Inglis'
_chemical_formula_moiety
'[Mn6Tb2O3(acac)2(MeSaO)6(MeO)4(MeOH)3(EtOH)].0.5H2O'
_chemical_formula_sum            'C67 H87 Mn6 N6 O27.5 Tb2'
_chemical_formula_weight         2063.87
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-02-04
_audit_creation_method           CRYSTALS_ver_14.05
_cell_angle_alpha                90
_cell_angle_beta                 92.941(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7152(3)
_cell_length_b                   25.6100(9)
_cell_length_c                   23.8804(7)
_cell_measurement_reflns_used    16286
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      73.8768
_cell_measurement_theta_min      2.5295
_cell_volume                     7766.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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      100.0
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44617
_diffrn_reflns_theta_full        69.600
_diffrn_reflns_theta_max         74.042
_diffrn_reflns_theta_min         2.532
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4124
_exptl_crystal_recrystallization_method
;
Slow evaporation of a MeOH/MeCN solution
;
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.92
_refine_diff_density_min         -1.50
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0007
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         15241
_refine_ls_number_restraints     667
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.0033713
_refine_ls_shift/su_mean         1.0608300
_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:
505. 451. 141.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0637
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0637
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                12785
_reflns_number_total             15309
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.76
_oxford_diffrn_Wilson_scale      0.83
_oxford_refine_ls_r_factor_ref   0.0691
_oxford_refine_ls_scale          1.2480(15)
_oxford_reflns_number_all        15241
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'eb1013 in P2(1)/c'
_cod_data_source_file            c1dt10154d.txt
_cod_data_source_block           eb1013
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C67 H87 Mn6 N6 O27.50 Tb2'
_cod_database_code               7015847