Switching from antiferromagnetic to ferromagnetic coupling in heptanuclear [M(t)6M(c)](n+) complexes by going from an achiral to a chiral triplesalen ligand.
Mukherjee, Chandan; Hoeke, Veronika; Stammler, Anja; Bögge, Hartmut; Schnack, Jürgen; Glaser, Thorsten; Dalton transactions (Cambridge, England : 2003) 43 (2014) 9690–9703; doi:10.1039/c4dt00670d

data_7029874
_publ_section_title
;
 Switching from antiferromagnetic to ferromagnetic coupling in
 heptanuclear [M(t)6M(c)](n+) complexes by going from an achiral to a
 chiral triplesalen ligand.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9690
_journal_page_last               9703
_journal_paper_doi               10.1039/c4dt00670d
_journal_volume                  43
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C156 H204 N18 O12 Mn6 Fe 5(C4 H8 O2) , 2(Cl O4) , 4(C4 H8 O2)'
_chemical_formula_sum            'C192 H276 Cl2 Fe Mn6 N18 O38'
_chemical_formula_weight         3900.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.1459(10)
_cell_length_b                   28.1670(12)
_cell_length_c                   31.7049(13)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.36
_cell_volume                     20670.0(15)
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS)'
_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Bruker Kappa APEX II'
_diffrn_measurement_device_type  'four circle diffractometer'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'graphit monochromator'
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            62676
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.9088
_exptl_absorpt_correction_T_min  0.8609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             8272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;

The not coordinating four dioxane molecules could be partially located but 
were strongly disordered so that they could not be properly refined. 
Thus they were removed from the coordinate set and their scattering 
contribution determined and removed from the data set using the SQUEEZE
routine. The results from the original refinement of these positions 
and from SQUEEZE are in good agreement: The unit cell contains four 
solvent Dioxane molecules per formula unit, which are 
disordered in a volume, which would allow approximately the double 
amount of solvent molecules to be placed there. 

;
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1053
_refine_ls_number_reflns         17687
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.117
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                14792
_reflns_number_total             17687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00670d2.cif
_cod_data_source_block           g1861
_cod_depositor_comments
'Adding full bibliography for 7029873--7029874.cif.'
_cod_original_sg_symbol_H-M      C222(1)
_cod_database_code               7029874