Structural and Spectroscopic Features of Mono- and Binuclear Nickel(II) Complexes with Tetradentate N(amine)2S(thiolate)2 Ligation
Robert T. Stibrany; Stephen Fox; Parimal K. Bharadwaj; Harvey J. Schugar; Joseph A. Potenza; Inorganic Chemistry 44 (2005) 8234–8242; doi:10.1021/ic050114h

data_4309918
_publ_section_title
;
Structural and Spectroscopic Features of Mono- and Binuclear Nickel(II)
Complexes with Tetradentate N(amine)2S(thiolate)2 Ligation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8234
_journal_page_last               8242
_journal_paper_doi               10.1021/ic050114h
_journal_volume                  44
_journal_year                    2005
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C8 H12 N2 Ni O4 S2, C3 H12 N2, 3(O)'
_chemical_formula_sum            'C11 H24 N4 Ni O7 S2'
_chemical_formula_weight         447.17
_chemical_name_systematic
; 
  N,N'-bis(1-carboxy-2-mercaptoethyl)-1,2-diaminoethanenickel(II)
 N,N'-1,3-diammoniumpropane 3 water solvate 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0080(16)
_cell_length_b                   13.371(3)
_cell_length_c                   18.151(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      21.79
_cell_measurement_theta_min      13.17
_cell_volume                     1943.5(7)
_computing_cell_refinement       'Enraf-Nonius SDP (1985)'
_computing_data_collection       'Enraf-Nonius SDP (1985)'
_computing_data_reduction        'CAD-4-PC (Enraf-Nonius, 1993)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996), ORTEP32 (Farrugia, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0119
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2041
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      1.53(1)
_exptl_crystal_density_method    'floatation in carbon tetrachloride/heptane'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         1976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+0.2151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1071
_reflns_number_gt                1675
_reflns_number_total             1976
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic050114hsi20050124_040612_2.cif
_cod_data_source_block           Ni(R,R-1)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4309918