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_4311587
_publ_section_title
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 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            'C14 H30 N2 Ni2 O2 S4'
_chemical_formula_weight         504.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yac'
_symmetry_space_group_name_H-M   'C 1 2/n 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                 99.07(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.842(5)
_cell_length_b                   5.9083(10)
_cell_length_c                   23.241(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      8
_cell_measurement_theta_min      5
_cell_volume                     2012.5(8)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius 1998)'
_computing_data_collection       'CAD4 Express (Enraf Nonius 1998)'
_computing_data_reduction        'Reduce (T. Luegger 1998)'
_computing_molecular_graphics
;
  ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.452
_diffrn_measured_fraction_theta_max 0.452
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'omega / 2 theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0.001
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            1828
_diffrn_reflns_theta_full        24.94
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.296
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0029(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.7086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                1462
_reflns_number_total             1754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0491940si20040621_124825.cif
_cod_data_source_block           complex5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.7086P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.7086P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4311587