#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/26/7112631.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_7112631
loop_
_publ_author_name
'Davin Tan'
'Vjekoslav Strukil'
'Cristina Mottillo'
'Tomislav Friscic'
_publ_section_title
;
 Mechanosynthesis of pharmaceutically relevant sulfonyl-(thio)ureas
;
_journal_name_full               Chem.Commun.
_journal_page_first              5248
_journal_paper_doi               10.1039/C3CC47905F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '2(C14 H12 N3 O4 S2), 2.5(C3 H6 O1), K2'
_chemical_formula_sum            'C35.5 H39 K2 N6 O10.5 S4'
_chemical_formula_weight         924.17
_chemical_name_common
'Potassium (4-nitrophenylcarbamothioyl)(tosyl)amide'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.650(2)
_cell_angle_beta                 93.736(2)
_cell_angle_gamma                96.762(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3664(12)
_cell_length_b                   16.466(3)
_cell_length_c                   18.699(3)
_cell_measurement_reflns_used    2340
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.26
_cell_measurement_theta_min      2.30
_cell_volume                     2134.1(6)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21256
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         1.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         7955
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0741P)²+0.0107P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                3987
_reflns_number_total             7955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47905f.txt
_cod_data_source_block           cm44_0m
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C35.50 H39 K2 N6 O10.50 S4'
_cod_database_code               7112631
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -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
O1 O 1.0433(4) 0.99159(18) 0.27155(16) 0.0445(8) Uani 1 1 d .
O2 O 0.7167(4) 0.98865(19) 0.24673(18) 0.0524(9) Uani 1 1 d .
N1 N 0.8798(5) 0.8872(2) 0.14846(19) 0.0408(9) Uani 1 1 d .
N2 N 0.9284(5) 0.8773(2) 0.0263(2) 0.0469(10) Uani 1 1 d .
H1N H 0.9463 0.9057 -0.0049 0.056 Uiso 1 1 calc R
C8 C 0.9214(6) 0.9283(3) 0.0987(3) 0.0414(11) Uani 1 1 d .
C9 C 0.9120(6) 0.7878(3) -0.0070(2) 0.0409(11) Uani 1 1 d .
C14 C 0.9032(7) 0.7573(3) -0.0850(3) 0.0531(13) Uani 1 1 d .
H14 H 0.9026 0.7960 -0.1123 0.064 Uiso 1 1 calc R
C11 C 0.8961(7) 0.6427(3) -0.0055(3) 0.0592(14) Uani 1 1 d .
H11 H 0.8917 0.6031 0.0210 0.071 Uiso 1 1 calc R
C12 C 0.8920(6) 0.6149(3) -0.0825(3) 0.0431(11) Uani 1 1 d .
C13 C 0.8953(7) 0.6714(3) -0.1226(3) 0.0545(13) Uani 1 1 d .
H13 H 0.8923 0.6520 -0.1749 0.065 Uiso 1 1 calc R
C10 C 0.9068(7) 0.7293(3) 0.0327(3) 0.0588(14) Uani 1 1 d .
H10 H 0.9105 0.7484 0.0850 0.071 Uiso 1 1 calc R
N3 N 0.8864(6) 0.5229(3) -0.1209(3) 0.0599(12) Uani 1 1 d .
O4 O 0.9046(6) 0.5004(2) -0.1884(2) 0.0802(12) Uani 1 1 d .
O3 O 0.8642(6) 0.4727(2) -0.0849(2) 0.0858(13) Uani 1 1 d .
N4 N 1.4667(5) 1.7045(2) 0.6419(2) 0.0435(9) Uani 1 1 d .
N5 N 1.4074(5) 1.6984(2) 0.5181(2) 0.0529(11) Uani 1 1 d .
H2N H 1.4177 1.7267 0.4864 0.063 Uiso 1 1 calc R
C15 C 1.4662(6) 1.6722(3) 0.7695(3) 0.0410(11) Uani 1 1 d .
C17 C 1.3171(6) 1.6149(3) 0.4867(2) 0.0410(11) Uani 1 1 d .
C16 C 1.4846(7) 1.7450(3) 0.5910(3) 0.0494(12) Uani 1 1 d .
C18 C 1.3039(6) 1.5522(3) 0.5230(3) 0.0497(12) Uani 1 1 d .
H18 H 1.3548 1.5657 0.5727 0.060 Uiso 1 1 calc R
C20 C 1.1403(6) 1.4503(3) 0.4118(3) 0.0397(11) Uani 1 1 d .
C22 C 1.2380(7) 1.5920(3) 0.4113(3) 0.0493(12) Uani 1 1 d .
H22 H 1.2458 1.6331 0.3863 0.059 Uiso 1 1 calc R
C19 C 1.2159(6) 1.4708(3) 0.4853(3) 0.0482(12) Uani 1 1 d .
H19 H 1.2073 1.4291 0.5096 0.058 Uiso 1 1 calc R
C21 C 1.1498(6) 1.5105(3) 0.3743(3) 0.0496(12) Uani 1 1 d .
H21 H 1.0973 1.4961 0.3246 0.059 Uiso 1 1 calc R
O6 O 0.9827(5) 1.3454(2) 0.3069(2) 0.0655(10) Uani 1 1 d .
O5 O 1.0335(5) 1.3115(2) 0.40855(19) 0.0660(10) Uani 1 1 d .
N6 N 1.0464(5) 1.3637(2) 0.3731(2) 0.0486(10) Uani 1 1 d .
C24 C 1.4687(7) 1.5300(3) 0.7755(3) 0.0633(15) Uani 1 1 d .
H24 H 1.4935 1.4742 0.7538 0.076 Uiso 1 1 calc R
C27 C 1.3931(7) 1.6936(3) 0.8368(3) 0.0594(14) Uani 1 1 d .
H27 H 1.3645 1.7488 0.8579 0.071 Uiso 1 1 calc R
C23 C 1.5031(7) 1.5895(3) 0.7377(3) 0.0538(13) Uani 1 1 d .
H23 H 1.5506 1.5740 0.6913 0.065 Uiso 1 1 calc R
C25 C 1.3998(7) 1.5503(4) 0.8432(3) 0.0631(15) Uani 1 1 d .
C26 C 1.3618(8) 1.6325(4) 0.8735(3) 0.0695(16) Uani 1 1 d .
H26 H 1.3139 1.6477 0.9198 0.083 Uiso 1 1 calc R
C28 C 1.3662(9) 1.4851(4) 0.8852(4) 0.095(2) Uani 1 1 d .
H28A H 1.4042 1.4318 0.8571 0.142 Uiso 1 1 calc R
H28B H 1.2376 1.4756 0.8909 0.142 Uiso 1 1 calc R
H28C H 1.4355 1.5067 0.9340 0.142 Uiso 1 1 calc R
O7 O 1.7195(4) 1.7818(2) 0.74734(18) 0.0572(9) Uani 1 1 d .
O8 O 1.4125(4) 1.82049(19) 0.75833(18) 0.0553(9) Uani 1 1 d .
O9 O 1.2766(6) 1.8029(3) 0.4229(2) 0.0845(13) Uani 1 1 d .
O10 O 1.6666(6) 2.1517(3) 0.8123(3) 0.129(2) Uani 1 1 d .
C30 C 1.2189(8) 1.8681(4) 0.4556(3) 0.0673(16) Uani 1 1 d .
C33 C 1.6288(8) 2.2238(4) 0.8332(5) 0.088(2) Uani 1 1 d .
C31 C 1.1210(9) 1.8735(4) 0.5236(4) 0.103(2) Uani 1 1 d .
H31A H 1.1123 1.8192 0.5333 0.155 Uiso 1 1 calc R
H31B H 0.9998 1.8870 0.5152 0.155 Uiso 1 1 calc R
H31C H 1.1879 1.9177 0.5663 0.155 Uiso 1 1 calc R
C29 C 1.2482(10) 1.9435(4) 0.4285(4) 0.113(3) Uani 1 1 d .
H29A H 1.3133 1.9296 0.3845 0.170 Uiso 1 1 calc R
H29B H 1.3189 1.9910 0.4674 0.170 Uiso 1 1 calc R
H29C H 1.1315 1.9591 0.4160 0.170 Uiso 1 1 calc R
K1 K 2.05615(15) 1.84157(6) 0.71379(6) 0.0534(3) Uani 1 1 d .
K2 K 0.37265(14) 1.02189(7) 0.22068(7) 0.0562(3) Uani 1 1 d .
C1A C 1.6357(9) 2.2781(4) 0.7817(4) 0.104(2) Uani 1 1 d .
H1A1 H 1.6652 2.2449 0.7332 0.155 Uiso 1 1 calc R
H1A2 H 1.7282 2.3275 0.8027 0.155 Uiso 1 1 calc R
H1A3 H 1.5183 2.2966 0.7762 0.155 Uiso 1 1 calc R
C2A C 1.5775(11) 2.2633(5) 0.9089(5) 0.140(3) Uani 1 1 d .
H2A1 H 1.6017 2.2280 0.9399 0.210 Uiso 1 1 calc R
H2A2 H 1.4490 2.2685 0.9058 0.210 Uiso 1 1 calc R
H2A3 H 1.6482 2.3194 0.9307 0.210 Uiso 1 1 calc R
S1 S 0.87046(15) 0.94104(7) 0.23480(6) 0.0371(3) Uani 1 1 d .
S3 S 1.52487(16) 1.75425(7) 0.72843(6) 0.0412(3) Uani 1 1 d .
S5 S 0.9708(2) 1.03573(8) 0.11446(7) 0.0643(4) Uani 1 1 d .
S6 S 1.5897(2) 1.84571(8) 0.60148(8) 0.0737(5) Uani 1 1 d .
C5 C 0.8306(6) 0.8575(3) 0.2748(2) 0.0363(10) Uani 1 1 d .
C3 C 0.7158(7) 0.8118(4) 0.3753(3) 0.0641(15) Uani 1 1 d .
H3 H 0.6518 0.8224 0.4177 0.077 Uiso 1 1 calc R
C7 C 0.8926(7) 0.7250(3) 0.2908(3) 0.0583(14) Uani 1 1 d .
H7 H 0.9482 0.6756 0.2749 0.070 Uiso 1 1 calc R
C6 C 0.9106(6) 0.7838(3) 0.2522(3) 0.0528(13) Uani 1 1 d .
H6 H 0.9771 0.7737 0.2106 0.063 Uiso 1 1 calc R
C2 C 0.7953(7) 0.7371(3) 0.3521(3) 0.0553(14) Uani 1 1 d .
C4 C 0.7315(7) 0.8712(3) 0.3354(3) 0.0568(14) Uani 1 1 d .
H4 H 0.6742 0.9202 0.3502 0.068 Uiso 1 1 calc R
C1 C 0.7766(8) 0.6726(4) 0.3953(3) 0.0849(19) Uani 1 1 d .
H1A H 0.7039 0.6924 0.4362 0.127 Uiso 1 1 calc R
H1B H 0.8964 0.6668 0.4150 0.127 Uiso 1 1 calc R
H1C H 0.7178 0.6178 0.3621 0.127 Uiso 1 1 calc R
C1S C 0.5000 1.0000 0.0000 0.181(8) Uani 1 2 d SDU
C2S C 0.444(3) 0.934(2) 0.034(2) 0.179(10) Uani 0.50 1 d PDU
H2S1 H 0.4471 0.8780 -0.0020 0.269 Uiso 0.50 1 calc PR
H2S2 H 0.3219 0.9378 0.0477 0.269 Uiso 0.50 1 calc PR
H2S3 H 0.5272 0.9411 0.0778 0.269 Uiso 0.50 1 calc PR
O1S O 0.506(4) 1.0783(7) 0.0351(19) 0.209(8) Uani 0.50 1 d PDU
C3S C 0.569(3) 0.965(3) -0.0722(7) 0.167(10) Uani 0.50 1 d PDU
H3S1 H 0.5465 0.9031 -0.0875 0.250 Uiso 0.50 1 calc PR
H3S2 H 0.6994 0.9836 -0.0676 0.250 Uiso 0.50 1 calc PR
H3S3 H 0.5085 0.9847 -0.1094 0.250 Uiso 0.50 1 calc PR
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'
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'
S S 0.1246 0.1234 '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'
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 O1 K2 132.63(17) . 1_655
S1 O1 K1 97.95(15) . 2_886
K2 O1 K1 95.52(9) 1_655 2_886
S1 O2 K2 156.7(2) . .
S1 O2 K1 94.66(15) . 2_886
K2 O2 K1 103.69(10) . 2_886
C8 N1 S1 120.0(3) . .
C8 N2 C9 132.7(4) . .
N1 C8 N2 116.1(4) . .
N1 C8 S5 128.0(3) . .
N2 C8 S5 115.9(3) . .
C10 C9 C14 118.7(4) . .
C10 C9 N2 124.4(4) . .
C14 C9 N2 116.9(4) . .
C13 C14 C9 121.4(4) . .
C12 C11 C10 120.0(4) . .
C13 C12 C11 121.1(4) . .
C13 C12 N3 120.4(4) . .
C11 C12 N3 118.5(4) . .
C12 C13 C14 119.0(5) . .
C11 C10 C9 119.8(5) . .
O3 N3 O4 123.3(4) . .
O3 N3 C12 119.1(5) . .
O4 N3 C12 117.6(4) . .
C16 N4 S3 120.5(3) . .
C17 N5 C16 132.3(4) . .
C27 C15 C23 119.8(4) . .
C27 C15 S3 118.5(4) . .
C23 C15 S3 121.7(4) . .
N5 C17 C18 125.2(4) . .
N5 C17 C22 116.4(4) . .
C18 C17 C22 118.3(4) . .
N4 C16 N5 115.7(4) . .
N4 C16 S6 129.4(4) . .
N5 C16 S6 114.9(3) . .
C19 C18 C17 120.0(4) . .
C21 C20 C19 121.3(4) . .
C21 C20 N6 119.3(4) . .
C19 C20 N6 119.4(4) . .
C21 C22 C17 121.2(4) . .
C18 C19 C20 120.4(4) . .
C22 C21 C20 118.8(4) . .
N6 O6 K1 92.1(3) . 2_886
N6 O5 K1 99.0(3) . 2_886
O6 N6 O5 122.7(4) . .
O6 N6 C20 119.0(4) . .
O5 N6 C20 118.3(4) . .
O6 N6 K1 65.7(2) . 2_886
O5 N6 K1 59.0(2) . 2_886
C20 N6 K1 165.3(3) . 2_886
C25 C24 C23 122.1(5) . .
C15 C27 C26 119.6(5) . .
C24 C23 C15 119.2(5) . .
C24 C25 C26 117.9(5) . .
C24 C25 C28 121.8(6) . .
C26 C25 C28 120.3(6) . .
C25 C26 C27 121.5(5) . .
S3 O7 K1 151.43(19) . .
S3 O7 K2 86.65(15) . 2_786
K1 O7 K2 86.35(9) . 2_786
S3 O8 K2 107.12(16) . 2_786
S3 O8 K1 132.39(19) . 1_455
K2 O8 K1 105.50(10) 2_786 1_455
C33 O10 K2 159.2(4) . 2_786
O9 C30 C29 119.7(6) . .
O9 C30 C31 120.5(6) . .
C29 C30 C31 119.9(6) . .
O10 C33 C2A 122.8(8) . .
O10 C33 C1A 120.5(8) . .
C2A C33 C1A 116.7(6) . .
O7 K1 O8 131.75(10) . 1_655
O7 K1 O5 80.13(10) . 2_886
O8 K1 O5 98.69(10) 1_655 2_886
O7 K1 O1 92.66(9) . 2_886
O8 K1 O1 121.64(9) 1_655 2_886
O5 K1 O1 128.77(10) 2_886 2_886
O7 K1 O2 134.89(10) . 2_886
O8 K1 O2 73.05(9) 1_655 2_886
O5 K1 O2 139.94(10) 2_886 2_886
O1 K1 O2 49.09(8) 2_886 2_886
O7 K1 O6 68.42(10) . 2_886
O8 K1 O6 77.77(10) 1_655 2_886
O5 K1 O6 43.81(10) 2_886 2_886
O1 K1 O6 159.89(10) 2_886 2_886
O2 K1 O6 150.78(10) 2_886 2_886
O7 K1 N6 70.08(10) . 2_886
O8 K1 N6 90.94(10) 1_655 2_886
O5 K1 N6 22.05(9) 2_886 2_886
O1 K1 N6 145.39(11) 2_886 2_886
O2 K1 N6 154.97(10) 2_886 2_886
O6 K1 N6 22.19(9) 2_886 2_886
O7 K1 S5 75.87(8) . 2_886
O8 K1 S5 89.32(8) 1_655 2_886
O5 K1 S5 153.61(8) 2_886 2_886
O1 K1 S5 63.82(6) 2_886 2_886
O2 K1 S5 66.45(7) 2_886 2_886
O6 K1 S5 115.22(8) 2_886 2_886
N6 K1 S5 134.01(9) 2_886 2_886
O7 K1 S1 111.62(8) . 2_886
O8 K1 S1 96.71(7) 1_655 2_886
O5 K1 S1 145.01(8) 2_886 2_886
O1 K1 S1 24.97(6) 2_886 2_886
O2 K1 S1 25.20(6) 2_886 2_886
O6 K1 S1 171.01(8) 2_886 2_886
N6 K1 S1 166.79(9) 2_886 2_886
S5 K1 S1 57.14(3) 2_886 2_886
O7 K1 K2 52.14(7) . 2_786
O8 K1 K2 144.17(7) 1_655 2_786
O5 K1 K2 115.84(8) 2_886 2_786
O1 K1 K2 40.80(6) 2_886 2_786
O2 K1 K2 85.38(6) 2_886 2_786
O6 K1 K2 120.54(8) 2_886 2_786
N6 K1 K2 117.41(7) 2_886 2_786
S5 K1 K2 55.47(4) 2_886 2_786
S1 K1 K2 60.47(3) 2_886 2_786
O7 K1 K2 152.30(8) . 2_886
O8 K1 K2 37.14(6) 1_655 2_886
O5 K1 K2 122.13(8) 2_886 2_886
O1 K1 K2 85.31(6) 2_886 2_886
O2 K1 K2 36.23(6) 2_886 2_886
O6 K1 K2 114.58(8) 2_886 2_886
N6 K1 K2 123.85(8) 2_886 2_886
S5 K1 K2 78.51(4) 2_886 2_886
S1 K1 K2 60.90(3) 2_886 2_886
K2 K1 K2 118.59(3) 2_786 2_886
O2 K2 O1 136.07(10) . 1_455
O2 K2 O10 75.78(12) . 2_786
O1 K2 O10 79.34(12) 1_455 2_786
O2 K2 O8 77.10(10) . 2_786
O1 K2 O8 128.14(9) 1_455 2_786
O10 K2 O8 151.15(12) 2_786 2_786
O2 K2 C3S 93.5(5) . 2_675
O1 K2 C3S 126.2(5) 1_455 2_675
O10 K2 C3S 99.4(8) 2_786 2_675
O8 K2 C3S 72.6(8) 2_786 2_675
O2 K2 O7 121.93(9) . 2_786
O1 K2 O7 84.94(8) 1_455 2_786
O10 K2 O7 162.11(12) 2_786 2_786
O8 K2 O7 46.45(8) 2_786 2_786
C3S K2 O7 83.0(8) 2_675 2_786
O2 K2 S6 88.93(8) . 2_786
O1 K2 S6 74.52(7) 1_455 2_786
O10 K2 S6 122.13(14) 2_786 2_786
O8 K2 S6 66.70(7) 2_786 2_786
C3S K2 S6 137.5(8) 2_675 2_786
O7 K2 S6 60.45(6) 2_786 2_786
O2 K2 C2S 83.3(4) . .
O1 K2 C2S 122.0(4) 1_455 .
O10 K2 C2S 71.7(3) 2_786 .
O8 K2 C2S 95.5(3) 2_786 .
C3S K2 C2S 27.9(6) 2_675 .
O7 K2 C2S 110.5(3) 2_786 .
S6 K2 C2S 161.9(3) 2_786 .
O2 K2 S3 97.68(7) . 2_786
O1 K2 S3 105.22(7) 1_455 2_786
O10 K2 S3 173.38(11) 2_786 2_786
O8 K2 S3 23.32(6) 2_786 2_786
C3S K2 S3 81.9(8) 2_675 2_786
O7 K2 S3 24.29(5) 2_786 2_786
S6 K2 S3 55.84(3) 2_786 2_786
C2S K2 S3 109.0(3) . 2_786
O2 K2 S5 157.54(8) . 1_455
O1 K2 S5 61.40(7) 1_455 1_455
O10 K2 S5 98.40(12) 2_786 1_455
O8 K2 S5 102.94(8) 2_786 1_455
C3S K2 S5 65.7(4) 2_675 1_455
O7 K2 S5 66.25(6) 2_786 1_455
S6 K2 S5 111.96(5) 2_786 1_455
C2S K2 S5 74.4(4) . 1_455
S3 K2 S5 88.07(4) 2_786 1_455
O2 K2 K1 150.98(8) . 2_786
O1 K2 K1 43.68(6) 1_455 2_786
O10 K2 K1 121.69(10) 2_786 2_786
O8 K2 K1 87.07(7) 2_786 2_786
C3S K2 K1 104.9(6) 2_675 2_786
O7 K2 K1 41.51(5) 2_786 2_786
S6 K2 K1 62.34(4) 2_786 2_786
C2S K2 K1 122.8(4) . 2_786
S3 K2 K1 63.82(3) 2_786 2_786
S5 K2 K1 49.79(3) 1_455 2_786
O2 K2 K1 40.08(7) . 2_886
O1 K2 K1 144.63(7) 1_455 2_886
O10 K2 K1 115.78(10) 2_786 2_886
O8 K2 K1 37.36(7) 2_786 2_886
C3S K2 K1 84.7(5) 2_675 2_886
O7 K2 K1 82.05(6) 2_786 2_886
S6 K2 K1 70.43(4) 2_786 2_886
C2S K2 K1 93.4(4) . 2_886
S3 K2 K1 57.76(3) 2_786 2_886
S5 K2 K1 138.17(4) 1_455 2_886
K1 K2 K1 118.59(3) 2_786 2_886
O1 S1 O2 113.54(19) . .
O1 S1 N1 113.28(18) . .
O2 S1 N1 113.9(2) . .
O1 S1 C5 106.52(19) . .
O2 S1 C5 107.41(19) . .
N1 S1 C5 100.98(19) . .
O1 S1 K1 57.07(12) . 2_886
O2 S1 K1 60.14(13) . 2_886
N1 S1 K1 118.71(13) . 2_886
C5 S1 K1 140.23(15) . 2_886
O7 S3 O8 114.5(2) . .
O7 S3 N4 114.04(19) . .
O8 S3 N4 112.3(2) . .
O7 S3 C15 106.7(2) . .
O8 S3 C15 106.6(2) . .
N4 S3 C15 101.5(2) . .
O7 S3 K2 69.05(14) . 2_786
O8 S3 K2 49.56(13) . 2_786
N4 S3 K2 116.64(14) . 2_786
C15 S3 K2 140.15(16) . 2_786
C8 S5 K1 116.04(16) . 2_886
C8 S5 K2 85.22(16) . 1_655
K1 S5 K2 74.74(4) 2_886 1_655
C16 S6 K2 113.40(17) . 2_786
C4 C5 C6 119.4(4) . .
C4 C5 S1 117.9(3) . .
C6 C5 S1 122.4(3) . .
C2 C3 C4 120.4(5) . .
C2 C7 C6 121.8(5) . .
C7 C6 C5 120.3(4) . .
C7 C2 C3 118.0(4) . .
C7 C2 C1 121.9(5) . .
C3 C2 C1 120.1(5) . .
C5 C4 C3 120.1(5) . .
O1S C1S O1S 180(3) 2_675 .
O1S C1S C3S 125.7(11) 2_675 2_675
O1S C1S C3S 54.3(11) . 2_675
O1S C1S C3S 54.3(11) 2_675 .
O1S C1S C3S 125.7(11) . .
C3S C1S C3S 180.0(6) 2_675 .
O1S C1S C2S 121.9(12) 2_675 2_675
O1S C1S C2S 58.1(12) . 2_675
C3S C1S C2S 111.9(12) 2_675 2_675
C3S C1S C2S 68.1(12) . 2_675
O1S C1S C2S 58.1(12) 2_675 .
O1S C1S C2S 121.9(12) . .
C3S C1S C2S 68.1(12) 2_675 .
C3S C1S C2S 111.9(12) . .
C2S C1S C2S 180(3) 2_675 .
C1S C2S K2 111(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 S1 1.441(3) .
O1 K2 2.710(3) 1_655
O1 K1 2.864(3) 2_886
O2 S1 1.443(3) .
O2 K2 2.699(3) .
O2 K1 2.941(3) 2_886
N1 C8 1.337(5) .
N1 S1 1.599(3) .
N2 C8 1.367(5) .
N2 C9 1.403(5) .
C8 S5 1.693(4) .
C9 C10 1.380(6) .
C9 C14 1.385(6) .
C14 C13 1.367(6) .
C11 C12 1.368(6) .
C11 C10 1.379(6) .
C12 C13 1.361(6) .
C12 N3 1.460(6) .
N3 O3 1.219(5) .
N3 O4 1.223(5) .
N4 C16 1.322(5) .
N4 S3 1.580(4) .
N5 C17 1.386(5) .
N5 C16 1.390(6) .
C15 C27 1.364(6) .
C15 C23 1.378(6) .
C15 S3 1.772(4) .
C17 C18 1.393(6) .
C17 C22 1.411(6) .
C16 S6 1.694(5) .
C18 C19 1.371(6) .
C20 C21 1.375(6) .
C20 C19 1.374(6) .
C20 N6 1.454(5) .
C22 C21 1.370(6) .
O6 N6 1.227(5) .
O6 K1 2.961(3) 2_886
O5 N6 1.234(5) .
O5 K1 2.817(3) 2_886
N6 K1 3.246(4) 2_886
C24 C25 1.357(7) .
C24 C23 1.382(6) .
C27 C26 1.386(7) .
C25 C26 1.370(7) .
C25 C28 1.517(7) .
O7 S3 1.439(3) .
O7 K1 2.741(3) .
O7 K2 3.266(3) 2_786
O8 S3 1.446(3) .
O8 K2 2.780(3) 2_786
O8 K1 2.794(3) 1_455
O9 C30 1.204(6) .
O10 C33 1.203(7) .
O10 K2 2.711(5) 2_786
C30 C29 1.476(7) .
C30 C31 1.488(8) .
C33 C2A 1.464(9) .
C33 C1A 1.499(9) .
K1 O8 2.794(3) 1_655
K1 O5 2.817(3) 2_886
K1 O1 2.864(3) 2_886
K1 O2 2.941(3) 2_886
K1 O6 2.961(3) 2_886
K1 N6 3.246(4) 2_886
K1 S5 3.2677(17) 2_886
K1 S1 3.3794(15) 2_886
K1 K2 4.1280(15) 2_786
K1 K2 4.4374(16) 2_886
K2 O1 2.710(3) 1_455
K2 O10 2.711(5) 2_786
K2 O8 2.780(3) 2_786
K2 C3S 2.90(2) 2_675
K2 O7 3.266(3) 2_786
K2 S6 3.3509(18) 2_786
K2 C2S 3.46(5) .
K2 S3 3.4909(16) 2_786
K2 S5 3.525(2) 1_455
K2 K1 4.1280(15) 2_786
K2 K1 4.4374(16) 2_886
S1 C5 1.759(4) .
S1 K1 3.3794(15) 2_886
S3 K2 3.4909(16) 2_786
S5 K1 3.2677(17) 2_886
S5 K2 3.525(2) 1_655
S6 K2 3.3509(18) 2_786
C5 C4 1.363(6) .
C5 C6 1.375(6) .
C3 C2 1.387(7) .
C3 C4 1.399(6) .
C7 C2 1.366(6) .
C7 C6 1.372(6) .
C2 C1 1.517(6) .
C1S O1S 1.2503(11) 2_675
C1S O1S 1.2503(11) .
C1S C3S 1.452(3) 2_675
C1S C3S 1.452(3) .
C1S C2S 1.452(3) 2_675
C1S C2S 1.452(3) .
