Bioinspired Enhancement of Superexchange: From 1,3,5-Trihydroxybenzene-Bridged to 1,3,5-Trimercaptobenzene-Bridged Trinuclear Copper(II) Complexes
Bastian Feldscher; Hubert Theil; Anja Stammler; Hartmut Bögge; Thorsten Glaser; Inorganic Chemistry 51 (2012) 8652–8654; doi:10.1021/ic301312v

data_4330115
_publ_contact_author_address
;     Fakult\"at f. Chemie
      Universit\"at Bielefeld
      33501 Bielefeld
      Germany
;
_publ_contact_author_email       thorsten.glaser@uni-bielefeld.de
_publ_contact_author_fax         '49 521 106 6003'
_publ_contact_author_name        'Prof. Dr. Thorsten. Glaser'
_publ_contact_author_phone       '49 521 106 6105'
_publ_section_title
;
 Bioinspired Enhancement of Superexchange: From
 1,3,5-Trihydroxybenzene-Bridged to 1,3,5-Trimercaptobenzene-Bridged
 Trinuclear Copper(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8652
_journal_page_last               8654
_journal_paper_doi               10.1021/ic301312v
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C69 H96 N6 O3 S3 Cu3 , 3(C H2 Cl2) , 6(C2 H3 N)'
_chemical_formula_sum            'C84 H120 Cl6 Cu3 N12 O3 S3'
_chemical_formula_weight         1845.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                120.00
_cell_formula_units_Z            8
_cell_length_a                   24.936(4)
_cell_length_b                   24.936(4)
_cell_length_c                   40.088(8)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.83
_cell_measurement_theta_min      2.20
_cell_volume                     21587(7)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'X8 PROSPECTOR ULTRA'
_diffrn_measurement_device_type  'three circle diffractometer'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'QuazarTM Montel Multilayer optics'
_diffrn_radiation_source         'I\mS Incoatec Microfocus Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            175349
_diffrn_reflns_theta_full        66.83
_diffrn_reflns_theta_max         66.83
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.942
_exptl_absorpt_correction_T_max  0.7191
_exptl_absorpt_correction_T_min  0.4930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Bruker AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       plate
_exptl_crystal_F_000             7752
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
 
 

Originally ca 1 CH2Cl2 and 5 MeCN molecules per complex were found but
did not refine properly due to severe disorder.
The electron count found by SQUEEZE after removal of the solvent
corresponds quite closely to 3 CH2Cl2 and 6 MeCN molecules, which are now
included in the sum formula and derived quantities.

;
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.046(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         25404
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+5.9040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                24301
_reflns_number_total             25404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301312v_si_002.cif
_cod_data_source_block           g2070
_cod_original_cell_volume        21588(6)
_cod_database_code               4330115