Structural influences on the exchange coupling and zero-field splitting in the single-molecule magnet [Mn(III)6Mn(III)]3+.
Hoeke, Veronika; Heidemeier, Maik; Krickemeyer, Erich; Stammler, Anja; Bögge, Hartmut; Schnack, Jürgen; Glaser, Thorsten; Dalton transactions (Cambridge, England : 2003) 41 (2012) 12942–12959; doi:10.1039/c2dt31590d

data_7029954
_publ_section_title
;
 Structural influences on the exchange coupling and zero-field splitting
 in the single-molecule magnet [Mn(III)6Mn(III)]3+.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12942
_journal_page_last               12959
_journal_paper_doi               10.1039/c2dt31590d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C237 H303 B3 Mn7 N21 O18'
_chemical_formula_weight         4151.01
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.780(2)
_cell_angle_beta                 78.080(3)
_cell_angle_gamma                77.748(3)
_cell_formula_units_Z            2
_cell_length_a                   18.6782(10)
_cell_length_b                   21.8337(11)
_cell_length_c                   31.2152(17)
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.91
_cell_volume                     12127.1(11)
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker KAPPA APEX II'
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            715193
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.9001
_exptl_absorpt_correction_T_min  0.8326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4412
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;

Originally 3Et2O, 3MeCN und 3MeOH molecules were found in the region of
the voids, but except 0.5 MeCN und 0.5 MeOH molecules could not properly be
refined due to severe disorder, and were therefore removed from the
coordinate set. The resulting void was then treated with "SQUEEZE" to
account for the now missing scattering power.
The removed molecules, however, are included in the given sum formula and thus
contribute to derived quantities like mu rho etc.

;
_refine_diff_density_max         1.323
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2566
_refine_ls_number_reflns         42619
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+22.7378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                35837
_reflns_number_total             42619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31590d.txt
_cod_data_source_block           g1887
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7029954