#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:54:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179942 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/37/7023769.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_7023769
loop_
_publ_author_name
'Imran, Muhammad'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Monkowius, Uwe'
'Ertl, Martin'
'Mitzel, Norbert W.'
_publ_section_title
;
 The versatile behaviour of a novel Janus scorpionate ligand towards
 sodium, potassium and bismuth(iii) ions.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15785
_journal_page_last               15795
_journal_paper_doi               10.1039/c3dt52030g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C18 H26 B2 K N18 Na S6'
_chemical_formula_sum            'C18 H26 B2 K N18 Na S6'
_chemical_formula_weight         770.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_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            2
_cell_length_a                   13.0298(7)
_cell_length_b                   13.0298(7)
_cell_length_c                   14.0697(9)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.290
_cell_measurement_theta_min      2.897
_cell_volume                     2068.7(2)
_computing_cell_refinement       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 v2009.11-0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Bruker KAPPA APEX II   '
_diffrn_measurement_device_type  'four three circle diffractometer'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'graphite monochromator  '
_diffrn_radiation_source         'fine focus sealed tube  '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            1560
_diffrn_reflns_theta_full        27.34
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.9248
_exptl_absorpt_correction_T_min  0.8139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0408P)²+6.7554P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                1442
_reflns_number_total             1560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52030g.txt
_cod_data_source_block           compound3a
_cod_database_code               7023769
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
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
K1 K 0.6667 0.3333 0.7500 0.0330(4) Uani 1 6 d S
S1 S 0.90128(8) 0.52373(8) 0.62933(7) 0.0308(3) Uani 1 1 d .
Na1 Na 0.6667 0.3333 0.2500 0.0476(11) Uani 1 6 d S
N1 N 0.7778(2) 0.4467(2) 0.46058(18) 0.0209(5) Uani 1 1 d .
N2 N 0.7889(3) 0.4821(3) 0.3670(2) 0.0319(7) Uani 1 1 d .
N3 N 0.9396(2) 0.6139(3) 0.4500(2) 0.0329(7) Uani 1 1 d .
B1 B 0.6667 0.3333 0.4963(4) 0.0190(11) Uani 1 3 d S
H1 H 0.6667 0.3333 0.5673 0.023 Uiso 1 3 calc SR
C1 C 0.8706(3) 0.5263(3) 0.5126(2) 0.0227(6) Uani 1 1 d .
C2 C 0.8881(3) 0.5832(4) 0.3638(3) 0.0378(9) Uani 1 1 d .
H2 H 0.9199 0.6292 0.3079 0.045 Uiso 1 1 calc R
C3 C 1.0531(3) 0.7193(4) 0.4699(4) 0.0496(12) Uani 1 1 d .
H3A H 1.0396 0.7804 0.4978 0.074 Uiso 1 1 calc R
H3B H 1.0980 0.7491 0.4107 0.074 Uiso 1 1 calc R
H3C H 1.0981 0.6993 0.5146 0.074 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
S1 K1 S1 98.34(3) 6_556 3_665
S1 K1 S1 95.72(2) 6_556 5_656
S1 K1 S1 162.53(3) 3_665 5_656
S1 K1 S1 162.53(3) 6_556 2_655
S1 K1 S1 95.72(2) 3_665 2_655
S1 K1 S1 72.65(3) 5_656 2_655
S1 K1 S1 95.72(2) 6_556 4_666
S1 K1 S1 72.65(3) 3_665 4_666
S1 K1 S1 95.72(2) 5_656 4_666
S1 K1 S1 98.34(3) 2_655 4_666
S1 K1 S1 72.65(3) 6_556 .
S1 K1 S1 95.72(2) 3_665 .
S1 K1 S1 98.34(3) 5_656 .
S1 K1 S1 95.72(2) 2_655 .
S1 K1 S1 162.53(3) 4_666 .
S1 K1 B1 121.108(15) 6_556 .
S1 K1 B1 58.892(15) 3_665 .
S1 K1 B1 121.108(15) 5_656 .
S1 K1 B1 58.892(15) 2_655 .
S1 K1 B1 121.108(15) 4_666 .
S1 K1 B1 58.892(15) . .
S1 K1 B1 58.892(15) 6_556 4_666
S1 K1 B1 121.108(15) 3_665 4_666
S1 K1 B1 58.892(15) 5_656 4_666
S1 K1 B1 121.108(15) 2_655 4_666
S1 K1 B1 58.892(15) 4_666 4_666
S1 K1 B1 121.109(15) . 4_666
B1 K1 B1 180.000(1) . 4_666
H1 K1 S1 121.1 . 6_556
H1 K1 S1 58.9 . 3_665
H1 K1 S1 121.1 . 5_656
H1 K1 S1 58.9 . 2_655
H1 K1 S1 121.1 . 4_666
H1 K1 S1 58.9 . .
H1 K1 B1 0.0 . .
H1 K1 B1 180.0 . 4_666
C1 S1 K1 112.08(11) . .
N2 Na1 N2 92.70(14) 6 3_665
N2 Na1 N2 79.23(10) 6 4_665
N2 Na1 N2 110.92(14) 3_665 4_665
N2 Na1 N2 110.92(14) 6 .
N2 Na1 N2 79.23(10) 3_665 .
N2 Na1 N2 165.84(15) 4_665 .
N2 Na1 N2 165.84(15) 6 2_655
N2 Na1 N2 79.23(10) 3_665 2_655
N2 Na1 N2 92.70(14) 4_665 2_655
N2 Na1 N2 79.23(10) . 2_655
N2 Na1 N2 79.23(10) 6 5_655
N2 Na1 N2 165.84(15) 3_665 5_655
N2 Na1 N2 79.23(10) 4_665 5_655
N2 Na1 N2 92.70(14) . 5_655
N2 Na1 N2 110.92(14) 2_655 5_655
C1 N1 N2 110.9(3) . .
C1 N1 B1 127.6(3) . .
N2 N1 B1 121.4(3) . .
C2 N2 N1 104.8(3) . .
C2 N2 Na1 134.8(3) . .
N1 N2 Na1 117.5(2) . .
C2 N3 C1 108.1(3) . .
C2 N3 C3 125.0(3) . .
C1 N3 C3 126.8(4) . .
N1 B1 N1 110.0(2) . 3_665
N1 B1 N1 110.0(2) . 2_655
N1 B1 N1 110.0(2) 3_665 2_655
N1 B1 K1 108.9(2) . .
N1 B1 K1 108.9(2) 3_665 .
N1 B1 K1 108.9(2) 2_655 .
N1 B1 H1 108.9 . .
N1 B1 H1 108.9 3_665 .
N1 B1 H1 108.9 2_655 .
K1 B1 H1 0.0 . .
N1 C1 N3 104.8(3) . .
N1 C1 S1 129.8(2) . .
N3 C1 S1 125.4(3) . .
N2 C2 N3 111.4(3) . .
N2 C2 H2 124.3 . .
N3 C2 H2 124.3 . .
N3 C3 H3A 109.5 . .
N3 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N3 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 S1 3.2860(9) 6_556
K1 S1 3.2860(9) 3_665
K1 S1 3.2860(9) 5_656
K1 S1 3.2860(9) 2_655
K1 S1 3.2860(9) 4_666
K1 S1 3.2860(9) .
K1 B1 3.570(6) .
K1 B1 3.570(6) 4_666
K1 H1 2.570 .
S1 C1 1.695(3) .
Na1 N2 2.432(3) 6
Na1 N2 2.432(3) 3_665
Na1 N2 2.432(3) 4_665
Na1 N2 2.432(3) .
Na1 N2 2.432(3) 2_655
Na1 N2 2.432(3) 5_655
N1 C1 1.349(4) .
N1 N2 1.379(4) .
N1 B1 1.546(3) .
N2 C2 1.307(5) .
N3 C2 1.346(5) .
N3 C1 1.364(4) .
N3 C3 1.456(5) .
B1 N1 1.546(3) 3_665
B1 N1 1.546(3) 2_655
B1 H1 1.0000 .
C2 H2 0.9500 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
