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_4322607
_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            'C16 H32 Br2 N2 Ni O1.5 S2'
_chemical_formula_weight         559.09
_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                 97.53(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.900(5)
_cell_length_b                   18.406(15)
_cell_length_c                   15.612(14)
_cell_measurement_temperature    163(2)
_cell_volume                     2251(3)
_computing_cell_refinement       'MSC CTR (4:1:0)'
_computing_data_collection       'MSC CTR (4:1:0)'
_computing_data_reduction        'MSC TEXSAN PROCESS'
_computing_molecular_graphics    'Siemens XP SHELXTL-PLUS'
_computing_publication_material  'SHELXL-93 CIFTAB'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measurement_device       'Rigaku AFC5'
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.7361
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3815
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.608
_exptl_absorpt_correction_type   difabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.997
_refine_ls_goodness_of_fit_obs   1.249
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         3765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_restrained_S_obs      1.249
_refine_ls_R_factor_all          0.4178
_refine_ls_R_factor_obs          0.1156
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0995P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3697
_refine_ls_wR_factor_obs         0.2153
_reflns_number_observed          1032
_reflns_number_total             3815
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970526t_1.cif
_cod_data_source_block           II*Br2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0995P)^2^+0.0000P] 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^)+( 0.0995P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2250.5(31)
_cod_original_formula_sum        'C16 H32 Br2 N2 Ni O1.50 S2'
_cod_database_code               4322607