Syntheses and Magnetostructural Investigations on Kuratowski-Type Homo- and Heteropentanuclear Coordination Compounds [MZn4Cl4(L)6] (MII= Zn, Fe, Co, Ni, or Cu; L = 5,6-Dimethyl-1,2,3-benzotriazolate) Represented by the Nonplanar K3,3 Graph
Shyam Biswas; Markus Tonigold; Manfred Speldrich; Paul Kögerler; Matthias Weil; Dirk Volkmer; Inorganic Chemistry 49 (2010) 7424–7434; doi:10.1021/ic100749k

data_4316246
_publ_contact_author_address
;Ulm University 
Institute of Inorganic Chemistry 2, Materials and Catalysis 
Albert-Einstein-Allee 11 
D-89081 Ulm 
Germany 
;
_publ_contact_author_email       dirk.volkmer@uni-ulm.de
_publ_contact_author_fax         '+49 (0)731/50-23039'
_publ_contact_author_name        'Professor Dirk Volkmer'
_publ_contact_author_phone       '+49 (0)731/50-23921'
_publ_section_title
;
 Syntheses and Magnetostructural Investigations on Kuratowski-Type Homo-
 and Heteropentanuclear Coordination Compounds [MZn4Cl4(L)6] (MII= Zn, Fe,
 Co, Ni, or Cu; L = 5,6-Dimethyl-1,2,3-benzotriazolate) Represented by the
 Nonplanar K3,3 Graph
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7424
_journal_page_last               7434
_journal_paper_doi               10.1021/ic100749k
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C48 H48 Cl4 N18 Ni Zn4, 2(C6 H5 Br1) '
_chemical_formula_sum            'C60 H58 Br2 Cl4 N18 Ni Zn4'
_chemical_formula_weight         1653.05
_chemical_name_systematic
; Hexakis(\m~3~-5,6-dimethyl-benzotriazolato)-

tetrakis(chlorido-zinc(II))-nickel(II) bromobenzene disolvate

;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      227
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_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            8
_cell_length_a                   23.7160(4)
_cell_length_b                   23.7160(4)
_cell_length_c                   23.7160(4)
_cell_measurement_reflns_used    54846
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      32.35
_cell_measurement_theta_min      2.43
_cell_volume                     13339.0(4)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD diffractometer'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0102
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54846
_diffrn_reflns_theta_full        32.35
_diffrn_reflns_theta_max         32.35
_diffrn_reflns_theta_min         2.43
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.107
_exptl_absorpt_correction_T_max  0.5226
_exptl_absorpt_correction_T_min  0.4009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

SADABS (Bruker, 2008)

;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'truncated octahedron'
_exptl_crystal_F_000             6640
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         1182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0276P)^2^+72.3040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                922
_reflns_number_total             1182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100749k_si_002_1.cif
_cod_data_source_block           4bNi
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_database_code               4316246