An Unsymmetrical Tripodal Ligand with NOS2-Donor Set: Coordination Chemistry with Nickel(II) and Zinc(II)
F. Ekkehardt Hahn; Christian Ochs; Thomas Lügger; Roland Fröhlich; Inorganic Chemistry 43 (2004) 6101–6107; doi:10.1021/ic0491940

data_4311588
_publ_section_title
;
 An Unsymmetrical Tripodal Ligand with NOS2-Donor Set: Coordination
 Chemistry with Nickel(II) and Zinc(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6101
_journal_page_last               6107
_journal_paper_doi               10.1021/ic0491940
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C28 H60 N4 O4 S8 Zn4'
_chemical_formula_weight         1034.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 104.31(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.594(1)
_cell_length_b                   12.531(1)
_cell_length_c                   23.022(1)
_cell_measurement_temperature    198(2)
_cell_volume                     4079.6(5)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Shedlrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27655
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  0.6813
_exptl_absorpt_correction_T_min  0.4902
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    'refined as riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         10028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+3.8230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                8583
_reflns_number_total             10028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0491940si20040621_124923.cif
_cod_data_source_block           complex6
_cod_database_code               4311588