#------------------------------------------------------------------------------
#$Date: 2021-05-16 12:36:21 +0300 (Sun, 16 May 2021) $
#$Revision: 265253 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/45/4324569.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_4324569
loop_
_publ_author_name
'Gernot Nuss'
'Gerald Saischek'
'Manuel Volpe'
'Karl Gatterer'
'Ferdinand Belaj'
'Nadia C. Mösch-Zanetti'
_publ_contact_author_address
; Institute of Chemistry,
  Karl-Franzens University Graz,
  Schubertstr. 1,
  A-8010 Graz,
  Austria
;
_publ_contact_author_email       ferdinand.belaj@uni-graz.at
_publ_contact_author_fax         43(316)3809835
_publ_contact_author_name        'Ferdinand Belaj'
_publ_contact_author_phone       43(316)3805288
_publ_section_title
;
 Novel Pyridazine Based Scorpionate Ligands in Cobalt and Nickel Boratrane
 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1991
_journal_page_last               2001
_journal_paper_doi               10.1021/ic102494k
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C15 H19 B K N6 O1.5 S3, 1.5(C H3 O H)'
_chemical_formula_sum            'C16.5 H25 B K N6 O3 S3'
_chemical_formula_weight         501.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            12
_cell_length_a                   13.7045(7)
_cell_length_b                   13.7045(7)
_cell_length_c                   45.762(4)
_cell_measurement_reflns_used    6194
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.47
_cell_volume                     7443.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            17144
_diffrn_reflns_theta_full        28.62
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       plate
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0736
_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)+(0.1289P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2402
_reflns_number_gt                2073
_reflns_number_total             3779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102494k_si_001_4.cif
_cod_data_source_block           pymebo
_cod_depositor_comments
;

2021-05-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C33 H50 B2 K2 N12 O6 S6'
_cod_original_formula_weight         1002.95
_cod_original_formula_moiety         'C30 H38 B2 K2 N12 O3 S6, 3(C H3 O H)'
_cod_original_formula_units_Z            6
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4324569
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.10233(4) 0.0377(4) Uani 1 3 d S
K2 K 0.6667 0.3333 -0.06062(5) 0.0476(5) Uani 1 3 d S
S1 S 0.52262(11) 0.40824(11) 0.14441(4) 0.0510(4) Uani 1 1 d .
S2 S 0.51218(9) 0.11574(9) 0.05933(3) 0.0334(3) Uani 1 1 d .
N1 N 0.5448(3) 0.2954(3) 0.18956(9) 0.0347(9) Uani 1 1 d .
N2 N 0.5130(4) 0.2307(4) 0.21390(10) 0.0510(12) Uani 1 1 d .
N3 N 0.6562(3) 0.2207(3) 0.01504(8) 0.0253(7) Uani 1 1 d .
N4 N 0.7158(3) 0.2275(3) -0.00950(8) 0.0304(8) Uani 1 1 d .
O1 O 0.5862(4) 0.4503(4) -0.08683(9) 0.0630(11) Uani 1 1 d .
B1 B 0.6667 0.3333 0.1795(2) 0.036(2) Uani 1 3 d S
H1J H 0.6667 0.3333 0.1576 0.043 Uiso 1 3 calc SR
B2 B 0.6667 0.3333 0.0258(2) 0.0256(16) Uani 1 3 d S
H2J H 0.6667 0.3333 0.0477 0.031 Uiso 1 3 calc SR
C1 C 0.4807(4) 0.3272(4) 0.17545(11) 0.0365(11) Uani 1 1 d .
C2 C 0.3696(4) 0.2866(4) 0.18654(12) 0.0428(12) Uani 1 1 d .
H2 H 0.3193 0.3049 0.1770 0.051 Uiso 1 1 calc R
C3 C 0.3369(4) 0.2215(4) 0.21089(13) 0.0455(12) Uani 1 1 d .
H3 H 0.2631 0.1932 0.2185 0.055 Uiso 1 1 calc R
C4 C 0.4113(5) 0.1968(5) 0.22437(13) 0.0509(13) Uani 1 1 d .
C5 C 0.3754(6) 0.1220(6) 0.25131(16) 0.081(2) Uani 1 1 d .
H5A H 0.4407 0.1447 0.2641 0.121 Uiso 1 1 calc R
H5B H 0.3451 0.0433 0.2454 0.121 Uiso 1 1 calc R
H5C H 0.3173 0.1296 0.2618 0.121 Uiso 1 1 calc R
C6 C 0.5964(3) 0.1244(3) 0.03099(10) 0.0275(9) Uani 1 1 d .
C7 C 0.6052(3) 0.0303(3) 0.02211(10) 0.0320(9) Uani 1 1 d .
H7 H 0.5673 -0.0378 0.0329 0.038 Uiso 1 1 calc R
C8 C 0.6665(3) 0.0356(3) -0.00142(11) 0.0320(9) Uani 1 1 d .
H8 H 0.6733 -0.0274 -0.0071 0.038 Uiso 1 1 calc R
C9 C 0.7208(3) 0.1378(3) -0.01760(10) 0.0293(9) Uani 1 1 d .
C10 C 0.7840(4) 0.1471(4) -0.04505(11) 0.0400(11) Uani 1 1 d .
H10A H 0.8036 0.2180 -0.0550 0.060 Uiso 1 1 calc R
H10B H 0.7367 0.0836 -0.0579 0.060 Uiso 1 1 calc R
H10C H 0.8529 0.1456 -0.0402 0.060 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
K K 0.2009 0.2494 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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'
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 88.82(5) . 2_655
S1 K1 S1 88.82(5) . 3_665
S1 K1 S1 88.82(5) 2_655 3_665
S1 K1 S2 114.77(3) . .
S1 K1 S2 75.95(3) 2_655 .
S1 K1 S2 151.13(3) 3_665 .
S1 K1 S2 151.13(3) . 2_655
S1 K1 S2 114.77(3) 2_655 2_655
S1 K1 S2 75.95(3) 3_665 2_655
S2 K1 S2 88.21(5) . 2_655
S1 K1 S2 75.95(3) . 3_665
S1 K1 S2 151.13(3) 2_655 3_665
S1 K1 S2 114.77(3) 3_665 3_665
S2 K1 S2 88.21(5) . 3_665
S2 K1 S2 88.20(5) 2_655 3_665
O1 K2 O1 101.03(12) 2_655 .
O1 K2 O1 101.03(12) 2_655 3_665
O1 K2 O1 101.03(12) . 3_665
O1 K2 N4 97.18(12) 2_655 3_665
O1 K2 N4 91.54(11) . 3_665
O1 K2 N4 155.36(13) 3_665 3_665
O1 K2 N4 91.54(11) 2_655 .
O1 K2 N4 155.36(13) . .
O1 K2 N4 97.18(12) 3_665 .
N4 K2 N4 65.70(11) 3_665 .
O1 K2 N4 155.36(13) 2_655 2_655
O1 K2 N4 97.18(12) . 2_655
O1 K2 N4 91.54(11) 3_665 2_655
N4 K2 N4 65.70(11) 3_665 2_655
N4 K2 N4 65.70(11) . 2_655
C1 S1 K1 110.09(16) . .
C6 S2 K1 106.55(14) . .
C1 N1 N2 124.5(4) . .
C1 N1 B1 121.6(4) . .
N2 N1 B1 113.9(4) . .
C4 N2 N1 117.9(4) . .
N4 N3 C6 123.8(3) . .
N4 N3 B2 115.9(4) . .
C6 N3 B2 120.1(4) . .
C9 N4 N3 118.4(4) . .
C9 N4 K2 111.1(3) . .
N3 N4 K2 113.8(2) . .
N1 B1 N1 111.6(4) 2_655 3_665
N1 B1 N1 111.6(4) 2_655 .
N1 B1 N1 111.6(4) 3_665 .
N3 B2 N3 110.5(3) 2_655 .
N3 B2 N3 110.5(3) 2_655 3_665
N3 B2 N3 110.5(3) . 3_665
N1 C1 C2 116.8(4) . .
N1 C1 S1 123.6(3) . .
C2 C1 S1 119.6(4) . .
C3 C2 C1 119.1(4) . .
C2 C3 C4 119.3(5) . .
N2 C4 C3 122.3(5) . .
N2 C4 C5 117.5(5) . .
C3 C4 C5 120.1(5) . .
N3 C6 C7 116.3(4) . .
N3 C6 S2 122.3(3) . .
C7 C6 S2 121.3(3) . .
C8 C7 C6 121.1(4) . .
C7 C8 C9 118.4(4) . .
N4 C9 C8 121.7(4) . .
N4 C9 C10 117.1(4) . .
C8 C9 C10 121.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 S1 3.2689(18) .
K1 S1 3.2689(18) 2_655
K1 S1 3.2690(18) 3_665
K1 S2 3.3067(16) .
K1 S2 3.3068(16) 2_655
K1 S2 3.3068(16) 3_665
K2 O1 2.644(4) 2_655
K2 O1 2.644(4) .
K2 O1 2.644(4) 3_665
K2 N4 3.001(4) 3_665
K2 N4 3.001(4) .
K2 N4 3.001(4) 2_655
S1 C1 1.716(5) .
S2 C6 1.700(4) .
N1 C1 1.326(6) .
N1 N2 1.353(5) .
N1 B1 1.551(5) .
N2 C4 1.319(7) .
N3 N4 1.364(5) .
N3 C6 1.365(5) .
N3 B2 1.558(4) .
N4 C9 1.318(5) .
B1 N1 1.551(5) 2_655
B1 N1 1.551(5) 3_665
B2 N3 1.558(4) 2_655
B2 N3 1.558(4) 3_665
C1 C2 1.427(6) .
C2 C3 1.356(7) .
C3 C4 1.371(8) .
C4 C5 1.520(8) .
C6 C7 1.414(6) .
C7 C8 1.344(6) .
C8 C9 1.422(6) .
C9 C10 1.494(6) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 184 39 ' '
2 0.333 0.667 0.167 319 49 ' '
3 0.000 0.000 0.500 318 49 ' '
4 -0.333 0.333 0.833 319 49 ' '
5 0.333 0.667 0.667 185 39 ' '
6 0.667 0.333 0.333 185 39 ' '
