9-(2-Carboxyphenyl)-3,6-bis(diethylamino)xanthylium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
Yuji Soneta; Shigeaki Sakamoto; Kazuo Miyamura; Acta Crystallographica Section E 62 (2006) m3448–m3450; doi:10.1107/S1600536806048148

data_2211405
_publ_section_title
;
 9-(2-Carboxyphenyl)-3,6-bis(diethylamino)xanthylium
 bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_journal_coeditor_code           GK2032
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3448
_journal_page_last               m3450
_journal_paper_doi               10.1107/S1600536806048148
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C28 H31 N2 O3 , C6 Ni S10'
_chemical_formula_moiety         'C28 H31 N2 O3 , C6 Ni S10'
_chemical_formula_sum            'C34 H31 N2 Ni O3 S10'
_chemical_formula_weight         894.92
_chemical_name_systematic
;
9-(2-Carboxyphenyl)-3,6-bis(diethylamino)xanthylium
bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III)
;
_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           SHELXL97
_cell_angle_alpha                105.729(7)
_cell_angle_beta                 96.342(7)
_cell_angle_gamma                91.138(8)
_cell_formula_units_Z            2
_cell_length_a                   10.187(4)
_cell_length_b                   10.752(4)
_cell_length_c                   18.285(7)
_cell_measurement_reflns_used    2181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      2.45
_cell_volume                     1913.4(13)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.1401
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11478
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  300
_diffrn_standards_number         60
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.7721
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(XPREP; Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.526
_refine_diff_density_min         -0.739
_refine_ls_extinction_coef       0.0052(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8212
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0878
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1434P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2700
_refine_ls_wR_factor_ref         0.2867
_reflns_number_gt                4839
_reflns_number_total             8212
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2032.cif
_cod_data_source_block           I
_cod_original_cell_volume        1913.5(13)
_cod_database_code               2211405
_cod_database_fobs_code          2211405