Bis(μ~2~-4,7-dimethyl-4,7-diazadecane-1,10-dithiolato)trinickel(II) bis(perchlorate)
Hirotsu, Masakazu; Kuwamura, Naoto; Kinoshita, Isamu; Kojima, Masaaki; Yoshikawa, Yuzo; Acta Crystallographica Section E 68 (2012) m307–; doi:10.1107/S1600536812006034

data_2233790
_publ_section_title
;
 Bis(\m~2~-4,7-dimethyl-4,7-diazadecane-1,10-dithiolato)trinickel(II)
 bis(perchlorate)
;
_journal_coeditor_code           FJ2508
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m307
_journal_paper_doi               10.1107/S1600536812006034
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni3 (C10 H22 N2 S2)2] (Cl O4)2'
_chemical_formula_moiety         'C20 H44 N4 Ni3 S4 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C20 H44 Cl2 N4 Ni3 O8 S4'
_chemical_formula_weight         843.83
_chemical_name_systematic
;
Bis(\m~2~-4,7-dimethyl-4,7-diazadecane-1,10-dithiolato)trinickel(II)
bis(perchlorate)
;
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 105.033(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   8.0253(19)
_cell_length_b                   16.208(4)
_cell_length_c                   12.807(3)
_cell_measurement_reflns_used    7222
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.1
_cell_volume                     1608.8(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
WinGX (Farrugia, 1999) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.1
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku AFC7 (Mercury CCD)'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15030
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    2.212
_exptl_absorpt_correction_T_max  0.7049
_exptl_absorpt_correction_T_min  0.6189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             876.00
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.710
_refine_diff_density_min         -0.704
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0319P)^2^+3.9221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                3391
_reflns_number_total             3626
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            fj2508.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C20 H44 Cl2 N4 Ni3 O8 S4 '
_cod_database_code               2233790
_cod_database_fobs_code          2233790