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_4321470
_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 Cu2 I4 N6 S4'
_chemical_formula_weight         1293.80
_chemical_name_systematic
;
[Cu~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                104.81(3)
_cell_angle_beta                 98.72(3)
_cell_angle_gamma                104.59(3)
_cell_formula_units_Z            1
_cell_length_a                   10.085(2)
_cell_length_b                   12.325(2)
_cell_length_c                   10.091(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1141.8(5)
_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-97-2 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'scintillation counter'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'theta-two theta'
_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  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3444
_diffrn_reflns_theta_full        22.97
_diffrn_reflns_theta_max         22.97
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        +/-0.2%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   'emprical, psi scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_meas      1.85(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       Tabloid
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.141
_refine_diff_density_min         -2.566
_refine_diff_density_rms         0.294
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    'H atoms not refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         3384
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.542
_refine_ls_shift/su_mean         0.090
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1712P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1947
_refine_ls_wR_factor_ref         0.2022
_reflns_number_gt                2974
_reflns_number_total             3384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000380p_2.cif
_cod_data_source_block           Meso-8
_cod_original_cell_volume        1141.7(4)
_cod_database_code               4321470