Crystal structure of bis[(18-crown-6)potassium] hexathiodiphosphate(V) acetonitrile disolvate, [K(C~12~H~24~O~6~)]~2~(P~2~S~6~) · 2CH~3~CN
Gjikaj, M.; Adam, A.; Duewel, M.; Brockner, W.; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 67–68; doi:

data_8101698
_publ_contact_author
;
Prof. Dr. W. Brockner
Institut f\"ur Anorganische und Analytische Chemie
Technische Universit\"at Clausthal
38678 Clausthal-Zellerfeld
Germany
;
_publ_contact_author_email       wolfgang.brockner@tu-clausthal.de
_publ_contact_author_phone       '049 5323 72-2656'
_publ_section_title
;
Crystal structure of bis[(18-crown-6)potassium] hexathiodiphosphate(V) 
acetonitrile disolvate, [K(C~12~H~24~O~6~)]~2~(P~2~S~6~) &#x00B7; 2CH~3~CN
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              67
_journal_page_last               68
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         '[K (18-crown-6)]2 [P2 S6] (C H 3 C N)2'
_chemical_formula_sum            'C28 H54 K2 N2 O12 P2 S6'
_chemical_formula_weight         943.24
_chemical_name_systematic
;
bis[potassium(18-crown-6)] hexathiodiphosphate(V) acetonitrile disolvate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.566(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.3073(8)
_cell_length_b                   17.070(2)
_cell_length_c                   16.176(2)
_cell_measurement_reflns_used    27487
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0.985
_cell_volume                     2283.0(4)
_computing_cell_refinement       'Stoe X-Area'
_computing_data_collection       'Stoe X-Area'
_computing_data_reduction        'Stoe X-Area'
_computing_molecular_graphics    'DIAMOND (Brandenburger, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997) [5]'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997) [5]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990) [5]'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method
;
rotation method at \f = 0\%, 45\", \D\w = 2\%
120 frames, detector distance 100 mm
;
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21155
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       compact
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.00046(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0353P)^2^+0.0837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                3567
_reflns_number_total             4901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1428.cff
_cod_data_source_block           K2[18-crown-6]2P2S6(MeCN)2
_cod_depositor_comments
;
The following corrections have been performed
in the original file before processing it for deposition
(the diff against the Z. Krist. - NCS original is given):

Index: 2005/01/1267-1428.cff
===================================================================
--- 2005/01/1267-1428.cff    (revision 562)
+++ 2005/01/1267-1428.cff    (revision 563)
@@ -1,3 +1,5 @@
+data_K2[18-crown-6]2P2S6(MeCN)2
+
 _audit_creation_method          'SHELXL-97 and manual editing'
 
@@ -131,8 +133,6 @@
 
-data_K2[18-crown-6]2P2S6(MeCN)2
-
 _symmetry_cell_setting                  monoclinic
 _symmetry_space_group_name_H-M          P121/c1
 

Saulius Gra\<zulis
2011-03-03
;
_cod_original_sg_symbol_H-M      P121/c1
_cod_original_formula_sum        'C14 H27 N O6 P S3 K'
_cod_database_code               8101698