Bis[2,5,8,11,14-pentaoxabicyclo[13.4.0]nonadeca-1(15),16,18-triene]potassium(I) bis(2-thioxo-4,5-dihydro-1,3-dithiole-4,5-dithiolato)nickel(III)
Jun-Hong Zhang; Da-Qi Wang; Jian-Min Dou; Acta Crystallographica Section E 61 (2005) m1699–m1700; doi:10.1107/S160053680502430X

data_2206822
_publ_section_title
;Bis[2,5,8,11,14-pentaoxabicyclo[13.4.0]nonadeca-1(15),16,18-triene]potassium(I)
 bis(2-thioxo-4,5-dihydro-1,3-dithiole-4,5-dithiolato)nickel(III)
;
_journal_coeditor_code           XU6034
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1699
_journal_page_last               m1700
_journal_paper_doi               10.1107/S160053680502430X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[K (C14 H20 O5)2] [Ni (C3 S5)2]'
_chemical_formula_moiety         'C28 H40 K O10 + , C6 Ni S10 -'
_chemical_formula_sum            'C34 H40 K Ni O10 S10'
_chemical_formula_weight         1027.07
_chemical_name_systematic
;bis[2,5,8,11,14-pentaoxabicyclo[13.4.0]nonadeca-1(15),16,18-triene]potassium(I)
bis(2-thioxo-4,5-dihydro-1,3-dithiole-4,5-dithiolato)nickel(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.648(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.270(6)
_cell_length_b                   11.800(4)
_cell_length_c                   21.927(8)
_cell_measurement_reflns_used    2431
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.143
_cell_measurement_theta_min      2.507
_cell_volume                     4424(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_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  0.074
_diffrn_reflns_av_sigmaI/netI    0.135
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22348
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.3
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2124
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7813
_refine_ls_number_restraints     1310
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.141
_refine_ls_R_factor_gt           0.047
_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^)] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.049
_refine_ls_wR_factor_ref         0.057
_reflns_number_gt                3106
_reflns_number_total             7813
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu6034.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2206822
_cod_database_fobs_code          2206822