Potassium bis(4,5-dimercapto-1,3-dithiole-2-thionato)nickelate 1,4,7,10,13,16-hexaoxa-2,3:11,12-dibenzocyclooctadeca-2,11-diene propanone solvate
Shitagami, Kozo; Akutagawa, Tomoyuki; Hasegawa, Tatsuo; Nakamura, Takayoshi; Robertson, Neil; Acta Crystallographica Section C 57 (2001) 1271–1273; doi:10.1107/S0108270101013713

data_2012336
_publ_section_title
;
 Potassium bis(4,5-dimercapto-1,3-dithiole-2-thionato)nickelate
 1,4,7,10,13,16-hexaoxa-2,3:11,12-dibenzocyclooctadeca-2,11-diene
 propanone solvate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1271
_journal_page_last               1273
_journal_paper_doi               10.1107/S0108270101013713
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'K [Ni (C3 S5)2] (C20 H24 O6), C3 H6 O1'
_chemical_formula_moiety         'K 1+, C6 Ni1 S10 1-, C20 H24 O6, C3 H6 O1'
_chemical_formula_sum            'C29 H30 K Ni O7 S10'
_chemical_formula_weight         908.95
_chemical_name_systematic
;
Potassium bis(4,5-dimercapto-1,3-dithiole-2-thionato)nickelate
2,3:11,12-dibenzo-1,4,7,10,13,16-hexaoxocyclooctadeca-2,11-diene
propanone solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.201(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.8232(5)
_cell_length_b                   22.4666(8)
_cell_length_c                   26.6120(10)
_cell_measurement_reflns_used    18032
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     7666.7(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_structure_refinement
'TEXSAN (Molecular Structure Corporation and Rigaku, 1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full .9977
_diffrn_measured_fraction_theta_max .9977
_diffrn_measurement_device       'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .7107
_diffrn_reflns_av_R_equivalents  .050
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            36400
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  .887
_exptl_absorpt_correction_T_min  .699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3736.00
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .35
_exptl_crystal_size_min          .10
_refine_diff_density_max         .32
_refine_diff_density_min         -.24
_refine_ls_extinction_coef       .0055(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4422
_refine_ls_R_factor_gt           .0349
_refine_ls_shift/su_max          .0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + {0.05[Max(Fo^2^,0) + 2Fc^2^]/3}^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .0877
_reflns_number_gt                4422
_reflns_number_total             8776
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            oa1119.cif
_cod_data_source_block           I
_cod_original_cell_volume        7666.6(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2012336
_cod_database_fobs_code          2012336