Square-Planar N2S2NiII Complexes with an Extended π-Conjugated System
Tatsuya Kawamoto; Kazunori Takeda; Masato Nishiwaki; Takashi Aridomi; Takumi Konno; Inorganic Chemistry 46 (2007) 4239–4247; doi:10.1021/ic0618246

data_4307283
_publ_section_title
;
Square-Planar N2S2NiII Complexes with an Extended \p-Conjugated System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4239
_journal_page_last               4247
_journal_paper_doi               10.1021/ic0618246
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C45 H29 Cl12 N5 O Ni S4 '
_chemical_formula_sum            'C45 H29 Cl12 N5 Ni O S4'
_chemical_formula_weight         1268.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.0(3)
_cell_angle_beta                 102.3(2)
_cell_angle_gamma                113.6(2)
_cell_formula_units_Z            2
_cell_length_a                   11.85(3)
_cell_length_b                   12.63(4)
_cell_length_c                   19.59(5)
_cell_measurement_reflns_used    9495
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      3.1
_cell_volume                     2576(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_sigmaI/netI    0.1761
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20230
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  -0.170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       0.0000(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         10088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.1704
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2467
_reflns_number_gt                3938
_reflns_number_total             10088
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0618246-file001_4.cif
_cod_data_source_block           3
_cod_original_cell_volume        2575(12)
_cod_database_code               4307283