Synthesis and Sulfur Oxygenation of a (N3S)Ni Complex Related to Nickel-Containing Superoxide Dismutase
Christopher S. Mullins; Craig A. Grapperhaus; Brian C. Frye; Larry H. Wood; Amy J. Hay; Robert M. Buchanan; Mark S. Mashuta; Inorganic Chemistry 48 (2009) 9974–9976; doi:10.1021/ic901246w

data_4303476
_publ_section_title
;
Synthesis and Sulfur Oxygenation of a (N3S)Ni Complex Related to
Nickel-Containing Superoxide Dismutase
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9974
_journal_page_last               9976
_journal_paper_doi               10.1021/ic901246w
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C11 H18 N4 Ni O S, H2 O'
_chemical_formula_sum            'C11 H20 N4 Ni O2 S'
_chemical_formula_weight         331.07
_chemical_name_common
; 
 (N-{2-[(2-mercapto-2-methylpropyl)amino]ethyl}-
 1-methylimidazole-2-carboxamido)nickel(II) 
;
_chemical_name_systematic
; 
 (N-{2-[(2-mercapto-2-methylpropyl)amino]ethyl}-
 1-methylimidazole-2-carboxamido)nickel(II) 
;
_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_date             'Jan 21, 2005'
_audit_creation_method           SHELXL-97
_audit_update_record
;
  Feb_22_2005 text and data added by Mark S. Mashuta
  March_31_2005 text and data added by Mark S. Mashuta
  April_4_2006 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.407(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.166(11)
_cell_length_b                   5.302(3)
_cell_length_c                   11.363(5)
_cell_measurement_reflns_used    4903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.55
_cell_volume                     1443.8(12)
_computing_cell_refinement       'SAINT 6.36 (Bruker, 2002)'
_computing_data_collection       'SMART 5.628 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36 (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11383
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, (1996).
;
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.102
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+1.8949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                2600
_reflns_number_total             3293
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic901246w_si_002_1.cif
_cod_data_source_block           1_cag109
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        1443.9(12)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C11 H20 N4 Ni1 O2 S1'
_cod_database_code               4303476