Synthesis, Structures, and Electrochemical Properties of Nickel Complexes of Macrocyclic N2S2 Aminothioethers
Ghezai Musie; Joseph H. Reibenspies; Marcetta Y. Darensbourg; Inorganic Chemistry 37 (1998) 302–310; doi:10.1021/ic970526t

data_4322608
_publ_section_title
;
 Synthesis, Structures, and Electrochemical Properties of Nickel Complexes
 of Macrocyclic N2S2 Aminothioethers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              302
_journal_page_last               310
_journal_paper_doi               10.1021/ic970526t
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C17 H39 Br2 N2 Ni O2.5 S2'
_chemical_formula_weight         594.15
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.84(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.821(5)
_cell_length_b                   7.848(2)
_cell_length_c                   32.968(8)
_cell_measurement_temperature    293(2)
_cell_volume                     4824(2)
_computing_cell_refinement       P3VAX
_computing_data_collection       P3VAX
_computing_data_reduction        XDISK
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.1884
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            8773
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    4.307
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_correction_T_min  0.6641
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.270
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00046(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.109
_refine_ls_goodness_of_fit_obs   1.403
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.951
_refine_ls_restrained_S_obs      1.403
_refine_ls_R_factor_all          0.1913
_refine_ls_R_factor_obs          0.0771
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;  
 calc [0.00000+1.00000exp(2.00(sinq/l)^2^)]/   
   [s^2^(Fo^2^)+ 0.0000+5.0000*P+(0.0435P)^2^+0.0000sinq/l]   
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3877
_refine_ls_wR_factor_obs         0.1247
_reflns_number_observed          3622
_reflns_number_total             8494
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970526t_2.cif
_cod_data_source_block           III*Br2
_cod_original_cell_volume        4824.1(21)
_cod_original_formula_sum        'C17 H39 Br2 N2 Ni O2.50 S2'
_cod_database_code               4322608