Copper(II) and Nickel(II) Complexes of Binucleating Macrocyclic Bis(disulfide)tetramine Ligands
Stephen Fox; Robert T. Stibrany; Joseph A. Potenza; Spencer Knapp; Harvey J. Schugar; Inorganic Chemistry 39 (2000) 4950–4961; doi:10.1021/ic000380p

data_4321471
_publ_section_title
;
 Copper(II) and Nickel(II) Complexes of Binucleating Macrocyclic
 Bis(disulfide)tetramine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4950
_journal_page_last               4961
_journal_paper_doi               10.1021/ic000380p
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C32 H62 I4 N6 Ni2 S4'
_chemical_formula_weight         1284.14
_chemical_name_systematic
;
 [Ni~2~(rac-9)I~2~(CH~3~CN)~2~]^2+^2I^-^
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.68(2)
_cell_angle_beta                 98.39(2)
_cell_angle_gamma                104.75(2)
_cell_formula_units_Z            1
_cell_length_a                   10.119(3)
_cell_length_b                   12.288(4)
_cell_length_c                   10.121(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1147.1(6)
_computing_cell_refinement       'Enraf-Nonius SDP (1983)'
_computing_data_collection       'Enraf-Nonius SDP (1983)'
_computing_data_reduction        'CAD-4/PC (Kretschmar, 1994)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(1)
_diffrn_measured_fraction_theta_full 0.546
_diffrn_measured_fraction_theta_max 0.546
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0116
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1577
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        +/-0.05%
_diffrn_standards_interval_time  '3 hours'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.724
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   'empirical psi scan'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Tabloid
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         1547
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          2.166
_refine_ls_shift/su_mean         0.133
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.6154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                1259
_reflns_number_total             1547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000380p_3.cif
_cod_data_source_block           Meso-7
_cod_database_code               4321471