Diazidobis[4,4,5,5-tetramethyl-2-(1,3-thiazol-2-yl)-2-imidazoline-1-oxyl 3-oxide-κ^2^<i>N</i>^1^,<i>O</i>^3^]nickel(II)
Chang, Jiu Li; Gao, Zhi Yong; Zhao, Ning; Acta Crystallographica Section E 66 (2010) m1481–; doi:10.1107/S1600536810042455

data_2227999
_publ_section_title
;
 Diazidobis[4,4,5,5-tetramethyl-2-(1,3-thiazol-2-yl)-2-imidazoline-1-oxyl
 3-oxide-\k^2^<i>N</i>^1^,<i>O</i>^3^]nickel(II)
;
_journal_coeditor_code           SJ5040
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1481
_journal_paper_doi               10.1107/S1600536810042455
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ni (N3)2 (C10 H14 N3 O2 S)2]'
_chemical_formula_moiety         'C20 H28 Ni N12 O4 S2'
_chemical_formula_sum            'C20 H28 N12 Ni O4 S2'
_chemical_formula_weight         623.37
_chemical_name_systematic
;
Diazidobis[4,4,5,5-tetramethyl-2-(1,3-thiazol-2-yl)-2-imidazoline-1-oxyl
3-oxide-\k^2^<i>N</i>^1^,<i>O</i>^3^]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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.6950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9212(7)
_cell_length_b                   12.1732(8)
_cell_length_c                   11.1795(8)
_cell_measurement_reflns_used    5712
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.26
_cell_measurement_theta_min      2.69
_cell_volume                     1317.17(16)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0098
_diffrn_reflns_av_sigmaI/netI    0.0109
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7812
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.8739
_exptl_absorpt_correction_T_min  0.7034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick , 1996)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0310P)^2^+0.5195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                2834
_reflns_number_total             3005
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5040.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2227999
_cod_database_fobs_code          2227999