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_7029873
_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 Fe7 3(C4 H8 O2)2(C H4 O) , 2(Cl O4) , 4(C4 H8 O2) , 2(C H4 O)'
_chemical_formula_sum            'C188 H276 Cl2 Fe7 N18 O38'
_chemical_formula_weight         3858.12
_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                   23.4878(16)
_cell_length_b                   28.214(2)
_cell_length_c                   31.304(2)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.26
_cell_volume                     20745(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            220880
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.8940
_exptl_absorpt_correction_T_min  0.8032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8200
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;

The not coordinating solvent 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 and two MeOH 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         0.870
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         18218
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1349P)^2^+9.0502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1744
_reflns_number_gt                15962
_reflns_number_total             18218
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00670d2.cif
_cod_data_source_block           g1858
_cod_depositor_comments
'Adding full bibliography for 7029873--7029874.cif.'
_cod_original_cell_volume        20745(3)
_cod_original_sg_symbol_H-M      C222(1)
_cod_database_code               7029873