#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:21:52 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179057 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/19/4301937.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4301937
loop_
_publ_author_name
'Sonja Tragl'
'Markus Ströbele'
'Jochen Glaser'
'Cristian Vicent'
'Rosa Llusar'
'H.-Jürgen Meyer'
_publ_contact_author
;
        H.-Juergen Meyer
        Institut fuer Anorganische Chemie
        Universitaet Tuebingen
        Ob dem Himmelreich 7
        72074 Tuebingen
        Bundesrepublik Deutschland
;
_publ_contact_author_email       juergen.meyer@uni-tuebingen.de
_publ_contact_author_fax         '07071 29-5702'
_publ_contact_author_phone       '07071 29-76226'
_publ_section_title
;
Compounds with the Electron-Rich [W6Cl18]2- Cluster Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3825
_journal_page_last               3831
_journal_paper_doi               10.1021/ic8019843
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'Cl18 K2 W6'
_chemical_formula_weight         1819.40
_chemical_name_systematic        ?
_space_group_IT_number           162
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2'
_symmetry_space_group_name_H-M   'P -3 1 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   9.3223(9)
_cell_length_b                   9.3223(9)
_cell_length_c                   8.4528(8)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      4.37
_cell_volume                     636.18(11)
_computing_cell_refinement       'Stoe IPDS software'
_computing_data_collection       'Stoe IPDS software'
_computing_data_reduction        'Stoe IPDS software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'phi scans'
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6779
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         4.37
_diffrn_standards_decay_%        0.01
_exptl_absorpt_coefficient_mu    29.222
_exptl_absorpt_correction_T_max  0.7336
_exptl_absorpt_correction_T_min  0.5137
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   X-Red/X-Shape
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.411
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     26
_refine_ls_number_reflns         507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0223
_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/[σ²(Fo²)+(0.0310P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                448
_reflns_number_total             507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8019843_si_001_5.cif
_cod_data_source_block           K2W6Cl18
_cod_database_code               4301937
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-y, -x, -z'
'-x+y, -x, z'
'x, x-y, -z'
'-x+y, y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'y, x, z'
'x-y, x, -z'
'-x, -x+y, z'
'x-y, -y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.0000 0.82006(3) 0.13777(4) 0.02338(14) Uani 1 2 d S . .
Cl1 Cl -0.2091(2) 0.7909(2) 0.3230(3) 0.0315(5) Uani 1 2 d S . .
Cl2 Cl 0.0000 0.6015(2) 0.3070(3) 0.0383(5) Uani 1 2 d S . .
Cl3 Cl -0.20962(13) 0.5808(3) 0.0000 0.0347(5) Uani 1 2 d S . .
K1 K -0.3333 0.3333 0.5000 0.0616(13) Uani 1 6 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.02617(19) 0.02143(16) 0.0241(2) 0.00210(11) 0.000 0.01308(10)
Cl1 0.0330(8) 0.0330(8) 0.0298(13) 0.0072(7) 0.0072(7) 0.0174(8)
Cl2 0.0501(13) 0.0322(8) 0.0386(14) 0.0097(8) 0.000 0.0250(7)
Cl3 0.0393(9) 0.0215(9) 0.0375(14) 0.000 -0.0056(8) 0.0107(4)
K1 0.0524(16) 0.0524(16) 0.080(4) 0.000 0.000 0.0262(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl3 W1 Cl3 89.366(15) 10_665 . ?
Cl3 W1 Cl1 88.49(6) 10_665 2_675 ?
Cl3 W1 Cl1 163.72(5) . 2_675 ?
Cl3 W1 Cl1 163.72(5) 10_665 . ?
Cl3 W1 Cl1 88.49(6) . . ?
Cl1 W1 Cl1 89.06(12) 2_675 . ?
Cl3 W1 Cl2 81.47(5) 10_665 . ?
Cl3 W1 Cl2 81.47(5) . . ?
Cl1 W1 Cl2 82.25(6) 2_675 . ?
Cl1 W1 Cl2 82.25(6) . . ?
Cl3 W1 W1 96.63(3) 10_665 8_455 ?
Cl3 W1 W1 53.39(3) . 8_455 ?
Cl1 W1 W1 142.88(3) 2_675 8_455 ?
Cl1 W1 W1 95.02(5) . 8_455 ?
Cl2 W1 W1 134.86(4) . 8_455 ?
Cl3 W1 W1 53.39(3) 10_665 3_665 ?
Cl3 W1 W1 96.63(3) . 3_665 ?
Cl1 W1 W1 95.02(5) 2_675 3_665 ?
Cl1 W1 W1 142.88(3) . 3_665 ?
Cl2 W1 W1 134.86(4) . 3_665 ?
W1 W1 W1 60.812(17) 8_455 3_665 ?
Cl3 W1 W1 95.71(2) 10_665 2_675 ?
Cl3 W1 W1 143.39(3) . 2_675 ?
Cl1 W1 W1 52.89(3) 2_675 2_675 ?
Cl1 W1 W1 95.62(5) . 2_675 ?
Cl2 W1 W1 135.14(4) . 2_675 ?
W1 W1 W1 90.0 8_455 2_675 ?
W1 W1 W1 59.594(9) 3_665 2_675 ?
Cl3 W1 W1 143.39(3) 10_665 9_465 ?
Cl3 W1 W1 95.71(2) . 9_465 ?
Cl1 W1 W1 95.62(5) 2_675 9_465 ?
Cl1 W1 W1 52.89(3) . 9_465 ?
Cl2 W1 W1 135.14(4) . 9_465 ?
W1 W1 W1 59.594(9) 8_455 9_465 ?
W1 W1 W1 90.0 3_665 9_465 ?
W1 W1 W1 60.0 2_675 9_465 ?
W1 Cl1 W1 74.23(7) . 9_465 ?
W1 Cl2 K1 121.40(4) . 7_566 ?
W1 Cl2 K1 121.40(4) . . ?
K1 Cl2 K1 109.95(7) 7_566 . ?
W1 Cl3 W1 73.22(6) . 8_455 ?
Cl2 K1 Cl2 97.58(9) 9_455 7_566 ?
Cl2 K1 Cl2 70.05(7) 9_455 3_556 ?
Cl2 K1 Cl2 97.48(6) 7_566 3_556 ?
Cl2 K1 Cl2 97.48(6) 9_455 . ?
Cl2 K1 Cl2 70.05(7) 7_566 . ?
Cl2 K1 Cl2 161.58(7) 3_556 . ?
Cl2 K1 Cl2 161.58(7) 9_455 8_456 ?
Cl2 K1 Cl2 97.48(6) 7_566 8_456 ?
Cl2 K1 Cl2 97.48(6) 3_556 8_456 ?
Cl2 K1 Cl2 97.58(9) . 8_456 ?
Cl2 K1 Cl2 97.48(6) 9_455 2_565 ?
Cl2 K1 Cl2 161.58(7) 7_566 2_565 ?
Cl2 K1 Cl2 97.58(9) 3_556 2_565 ?
Cl2 K1 Cl2 97.48(6) . 2_565 ?
Cl2 K1 Cl2 70.05(7) 8_456 2_565 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 Cl3 2.4066(17) 10_665 ?
W1 Cl3 2.4066(17) . ?
W1 Cl1 2.4075(18) 2_675 ?
W1 Cl1 2.4075(18) . ?
W1 Cl2 2.489(2) . ?
W1 W1 2.8703(6) 8_455 ?
W1 W1 2.8703(6) 3_665 ?
W1 W1 2.9054(6) 2_675 ?
W1 W1 2.9054(6) 9_465 ?
Cl1 W1 2.4075(18) 9_465 ?
Cl2 K1 3.2863(14) 7_566 ?
Cl2 K1 3.2863(14) . ?
Cl3 W1 2.4066(17) 8_455 ?
K1 Cl2 3.2863(14) 9_455 ?
K1 Cl2 3.2863(14) 7_566 ?
K1 Cl2 3.2863(14) 3_556 ?
K1 Cl2 3.2863(14) 8_456 ?
K1 Cl2 3.2863(14) 2_565 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl3 W1 Cl1 W1 179.13(16) 10_665 . . 9_465 ?
Cl3 W1 Cl1 W1 -98.33(6) . . . 9_465 ?
Cl1 W1 Cl1 W1 97.77(5) 2_675 . . 9_465 ?
Cl2 W1 Cl1 W1 -179.92(6) . . . 9_465 ?
W1 W1 Cl1 W1 -45.28(5) 8_455 . . 9_465 ?
W1 W1 Cl1 W1 0.67(13) 3_665 . . 9_465 ?
W1 W1 Cl1 W1 45.21(5) 2_675 . . 9_465 ?
Cl3 W1 Cl2 K1 61.07(8) 10_665 . . 7_566 ?
Cl3 W1 Cl2 K1 151.71(10) . . . 7_566 ?
Cl1 W1 Cl2 K1 -28.55(11) 2_675 . . 7_566 ?
Cl1 W1 Cl2 K1 -118.66(11) . . . 7_566 ?
W1 W1 Cl2 K1 151.96(5) 8_455 . . 7_566 ?
W1 W1 Cl2 K1 60.83(14) 3_665 . . 7_566 ?
W1 W1 Cl2 K1 -28.47(14) 2_675 . . 7_566 ?
W1 W1 Cl2 K1 -118.75(5) 9_465 . . 7_566 ?
Cl3 W1 Cl2 K1 -151.71(10) 10_665 . . . ?
Cl3 W1 Cl2 K1 -61.07(8) . . . . ?
Cl1 W1 Cl2 K1 118.66(11) 2_675 . . . ?
Cl1 W1 Cl2 K1 28.55(11) . . . . ?
W1 W1 Cl2 K1 -60.83(14) 8_455 . . . ?
W1 W1 Cl2 K1 -151.96(5) 3_665 . . . ?
W1 W1 Cl2 K1 118.75(5) 2_675 . . . ?
W1 W1 Cl2 K1 28.47(14) 9_465 . . . ?
Cl3 W1 Cl3 W1 -98.75(3) 10_665 . . 8_455 ?
Cl1 W1 Cl3 W1 178.8(2) 2_675 . . 8_455 ?
Cl1 W1 Cl3 W1 97.39(4) . . . 8_455 ?
Cl2 W1 Cl3 W1 179.79(5) . . . 8_455 ?
W1 W1 Cl3 W1 -45.736(10) 3_665 . . 8_455 ?
W1 W1 Cl3 W1 0.0 2_675 . . 8_455 ?
W1 W1 Cl3 W1 44.930(8) 9_465 . . 8_455 ?
W1 Cl2 K1 Cl2 114.07(5) . . . 9_455 ?
K1 Cl2 K1 Cl2 -95.39(11) 7_566 . . 9_455 ?
W1 Cl2 K1 Cl2 -150.55(16) . . . 7_566 ?
K1 Cl2 K1 Cl2 0.0 7_566 . . 7_566 ?
W1 Cl2 K1 Cl2 160.08(11) . . . 3_556 ?
K1 Cl2 K1 Cl2 -49.37(6) 7_566 . . 3_556 ?
W1 Cl2 K1 Cl2 -55.30(8) . . . 8_456 ?
K1 Cl2 K1 Cl2 95.25(8) 7_566 . . 8_456 ?
W1 Cl2 K1 Cl2 15.46(12) . . . 2_565 ?
K1 Cl2 K1 Cl2 166.00(6) 7_566 . . 2_565 ?
