#------------------------------------------------------------------------------
#$Date: 2017-07-11 15:10:40 +0300 (Tue, 11 Jul 2017) $
#$Revision: 198633 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/02/50/4025047.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_4025047
loop_
_publ_author_name
'Pedro Mateus'
'Rita Delgado'
'Paula Brandão'
'Vítor Félix'
_publ_contact_author_address
;Instituto de Tecnologia Química e Biológica,
UNL, Av. da República - EAN, 
2780-157 Oeiras, Portugal
;
_publ_contact_author_email       delgado@itqb.unl.pt
_publ_contact_author_fax         '(+351) 21 441 1277'
_publ_contact_author_name        'Rita Delgado'
_publ_contact_author_phone       '(+351) 21 446 9737'
_publ_section_title
;
Polyaza Cryptand Receptor Selective for Dihydrogen Phosphate
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8638
_journal_page_last               8646
_journal_paper_doi               10.1021/jo901742d
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C51 H95 N9 O26 S4'
_chemical_formula_weight         1378.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 91.517(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8516(17)
_cell_length_b                   15.2203(19)
_cell_length_c                   33.144(4)
_cell_measurement_temperature    150(2)
_cell_volume                     6480.9(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'PLATON (Spek, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            55877
_diffrn_reflns_theta_full        30.19
_diffrn_reflns_theta_max         30.19
_diffrn_reflns_theta_min         1.47
_diffrn_standards_interval_count 0.5
_diffrn_standards_interval_time  60
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.9861
_exptl_absorpt_correction_T_min  0.9591
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     879
_refine_ls_number_reflns         17270
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0892P)²+2.4660P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1553
_reflns_number_gt                12853
_reflns_number_total             17270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901742d_si_001_3.cif
_cod_data_source_block           SO4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+2.4660P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+2.4660P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4025047
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.94038(12) 0.14391(12) 0.26443(4) 0.0137(3) Uani 1 d . . .
H1A H 0.9217 0.2016 0.2602 0.016 Uiso 1 calc R . .
H1B H 0.8933 0.1088 0.2506 0.016 Uiso 1 calc R . .
N8 N 0.77055(12) 0.19388(12) 0.30239(4) 0.0140(3) Uani 1 d . . .
N10 N 0.60989(12) 0.22118(12) 0.24648(4) 0.0138(3) Uani 1 d . . .
H10A H 0.6098 0.1610 0.2492 0.017 Uiso 1 calc R . .
H10B H 0.6705 0.2372 0.2343 0.017 Uiso 1 calc R . .
N16 N 0.70840(12) 0.34832(12) 0.07706(4) 0.0130(3) Uani 1 d . . .
H16A H 0.7179 0.3750 0.1018 0.016 Uiso 1 calc R . .
H16B H 0.7596 0.3067 0.0743 0.016 Uiso 1 calc R . .
N23 N 0.89722(13) 0.43201(12) 0.06605(4) 0.0146(3) Uani 1 d . . .
N25 N 1.05205(13) 0.35154(12) 0.10703(5) 0.0154(3) Uani 1 d . . .
H25A H 1.0243 0.3120 0.0887 0.018 Uiso 1 calc R . .
H25B H 1.0018 0.3644 0.1254 0.018 Uiso 1 calc R . .
N35 N 0.98626(12) -0.02450(12) 0.09126(5) 0.0145(3) Uani 1 d . . .
H35A H 0.9337 -0.0273 0.1095 0.017 Uiso 1 calc R . .
H35B H 0.9757 0.0250 0.0758 0.017 Uiso 1 calc R . .
N42 N 0.80686(13) -0.12137(12) 0.08978(5) 0.0151(3) Uani 1 d . . .
N44 N 0.64249(12) -0.04985(12) 0.13843(5) 0.0135(3) Uani 1 d . . .
H44A H 0.6995 -0.0201 0.1292 0.016 Uiso 1 calc R . .
H44B H 0.6456 -0.0486 0.1662 0.016 Uiso 1 calc R . .
C2 C 0.93856(15) 0.12335(17) 0.30830(5) 0.0189(4) Uani 1 d . . .
H2A H 0.9951 0.1559 0.3226 0.023 Uiso 1 calc R . .
H2B H 0.9513 0.0598 0.3123 0.023 Uiso 1 calc R . .
C3 C 0.83616(15) 0.14759(14) 0.32597(5) 0.0142(4) Uani 1 d . . .
C4 C 0.81251(16) 0.12221(16) 0.36526(5) 0.0187(4) Uani 1 d . . .
H4 H 0.8613 0.0907 0.3817 0.022 Uiso 1 calc R . .
C5 C 0.71526(17) 0.14463(16) 0.37944(6) 0.0210(4) Uani 1 d . . .
H5 H 0.6968 0.1288 0.4060 0.025 Uiso 1 calc R . .
C6 C 0.64497(16) 0.19027(16) 0.35471(6) 0.0194(4) Uani 1 d . . .
H6 H 0.5775 0.2048 0.3636 0.023 Uiso 1 calc R . .
C7 C 0.67675(15) 0.21392(14) 0.31651(5) 0.0146(4) Uani 1 d . . .
C9 C 0.60605(15) 0.26306(15) 0.28744(5) 0.0174(4) Uani 1 d . . .
H9A H 0.5338 0.2618 0.2971 0.021 Uiso 1 calc R . .
H9B H 0.6285 0.3252 0.2858 0.021 Uiso 1 calc R . .
C11 C 0.51735(14) 0.24925(15) 0.22029(5) 0.0148(4) Uani 1 d . . .
H11A H 0.5118 0.3141 0.2202 0.018 Uiso 1 calc R . .
H11B H 0.4526 0.2250 0.2314 0.018 Uiso 1 calc R . .
C12 C 0.53025(14) 0.21639(14) 0.17749(5) 0.0128(4) Uani 1 d . . .
C13 C 0.55405(14) 0.27603(14) 0.14643(5) 0.0133(4) Uani 1 d . . .
C14 C 0.58215(14) 0.24195(14) 0.10865(5) 0.0130(4) Uani 1 d . . .
C15 C 0.60260(14) 0.30523(15) 0.07447(5) 0.0156(4) Uani 1 d . . .
H15A H 0.5959 0.2731 0.0486 0.019 Uiso 1 calc R . .
H15B H 0.5486 0.3516 0.0743 0.019 Uiso 1 calc R . .
C17 C 0.71513(16) 0.41465(15) 0.04438(6) 0.0187(4) Uani 1 d . . .
H17A H 0.6564 0.4563 0.0466 0.022 Uiso 1 calc R . .
H17B H 0.7072 0.3845 0.0180 0.022 Uiso 1 calc R . .
C18 C 0.81554(15) 0.46582(14) 0.04509(5) 0.0147(4) Uani 1 d . . .
C19 C 0.82100(16) 0.54425(15) 0.02327(5) 0.0167(4) Uani 1 d . . .
H19 H 0.7622 0.5657 0.0083 0.020 Uiso 1 calc R . .
C20 C 0.91470(17) 0.58994(15) 0.02402(6) 0.0183(4) Uani 1 d . . .
H20 H 0.9206 0.6440 0.0099 0.022 Uiso 1 calc R . .
C21 C 0.99925(16) 0.55581(15) 0.04548(6) 0.0180(4) Uani 1 d . . .
H21 H 1.0638 0.5862 0.0467 0.022 Uiso 1 calc R . .
C22 C 0.98725(15) 0.47583(15) 0.06520(5) 0.0149(4) Uani 1 d . . .
C24 C 1.08130(15) 0.43306(15) 0.08557(6) 0.0174(4) Uani 1 d . . .
H24A H 1.1333 0.4189 0.0650 0.021 Uiso 1 calc R . .
H24B H 1.1137 0.4748 0.1051 0.021 Uiso 1 calc R . .
C26 C 1.14450(15) 0.31043(15) 0.12880(6) 0.0176(4) Uani 1 d . . .
H26A H 1.1696 0.3503 0.1505 0.021 Uiso 1 calc R . .
H26B H 1.2016 0.3026 0.1096 0.021 Uiso 1 calc R . .
C27 C 1.11707(14) 0.22241(15) 0.14683(5) 0.0146(4) Uani 1 d . . .
C28 C 1.08560(14) 0.21842(14) 0.18710(5) 0.0135(4) Uani 1 d . . .
C29 C 1.06051(14) 0.13640(14) 0.20388(5) 0.0135(4) Uani 1 d . . .
C30 C 1.04817(14) 0.12824(15) 0.24914(5) 0.0151(4) Uani 1 d . . .
H30A H 1.0704 0.0685 0.2575 0.018 Uiso 1 calc R . .
H30B H 1.0962 0.1705 0.2626 0.018 Uiso 1 calc R . .
C31 C 1.05733(13) 0.06059(14) 0.17984(5) 0.0123(4) Uani 1 d . . .
C32 C 1.09053(14) 0.06552(14) 0.13974(5) 0.0134(4) Uani 1 d . . .
C33 C 1.12381(13) 0.14536(15) 0.12356(5) 0.0142(4) Uani 1 d . . .
C34 C 1.08933(14) -0.01669(15) 0.11386(5) 0.0159(4) Uani 1 d . . .
H34A H 1.1464 -0.0140 0.0944 0.019 Uiso 1 calc R . .
H34B H 1.1005 -0.0690 0.1312 0.019 Uiso 1 calc R . .
C36 C 0.98063(16) -0.10342(16) 0.06470(6) 0.0199(4) Uani 1 d . . .
H36A H 1.0222 -0.1515 0.0771 0.024 Uiso 1 calc R . .
H36B H 1.0107 -0.0893 0.0383 0.024 Uiso 1 calc R . .
C37 C 0.86910(15) -0.13346(14) 0.05837(5) 0.0149(4) Uani 1 d . . .
C38 C 0.83670(16) -0.17667(15) 0.02316(6) 0.0186(4) Uani 1 d . . .
H38 H 0.8827 -0.1839 0.0014 0.022 Uiso 1 calc R . .
C39 C 0.73596(17) -0.20875(17) 0.02059(6) 0.0220(5) Uani 1 d . . .
H39 H 0.7120 -0.2391 -0.0029 0.026 Uiso 1 calc R . .
C40 C 0.66994(16) -0.19624(16) 0.05277(6) 0.0193(4) Uani 1 d . . .
H40 H 0.6002 -0.2169 0.0515 0.023 Uiso 1 calc R . .
C41 C 0.70912(15) -0.15258(14) 0.08673(5) 0.0150(4) Uani 1 d . . .
C43 C 0.64682(16) -0.14344(14) 0.12441(6) 0.0168(4) Uani 1 d . . .
H43A H 0.5752 -0.1651 0.1190 0.020 Uiso 1 calc R . .
H43B H 0.6786 -0.1802 0.1461 0.020 Uiso 1 calc R . .
C45 C 0.54453(15) -0.00385(14) 0.12361(6) 0.0153(4) Uani 1 d . . .
H45A H 0.5349 -0.0136 0.0942 0.018 Uiso 1 calc R . .
H45B H 0.4838 -0.0292 0.1372 0.018 Uiso 1 calc R . .
C46 C 0.54974(14) 0.09359(14) 0.13197(5) 0.0137(4) Uani 1 d . . .
C47 C 0.58536(14) 0.15105(14) 0.10197(5) 0.0133(4) Uani 1 d . . .
C48 C 0.62141(15) 0.11429(16) 0.06199(5) 0.0179(4) Uani 1 d . . .
H48A H 0.6555 0.0568 0.0669 0.022 Uiso 1 calc R . .
H48B H 0.6739 0.1545 0.0508 0.022 Uiso 1 calc R . .
C49 C 0.53203(17) 0.10230(18) 0.03081(6) 0.0247(5) Uani 1 d . . .
H49A H 0.4810 0.0609 0.0413 0.030 Uiso 1 calc R . .
H49B H 0.5597 0.0792 0.0057 0.030 Uiso 1 calc R . .
H49C H 0.4984 0.1591 0.0256 0.030 Uiso 1 calc R . .
C50 C 0.51969(13) 0.12636(14) 0.16960(5) 0.0128(4) Uani 1 d . . .
C51 C 0.46712(15) 0.06759(15) 0.20029(6) 0.0162(4) Uani 1 d . . .
H51A H 0.4881 0.0866 0.2279 0.019 Uiso 1 calc R . .
H51B H 0.4908 0.0062 0.1967 0.019 Uiso 1 calc R . .
C52 C 0.34814(16) 0.07127(18) 0.19552(6) 0.0245(5) Uani 1 d . . .
H52A H 0.3253 0.1327 0.1955 0.029 Uiso 1 calc R . .
H52B H 0.3168 0.0401 0.2180 0.029 Uiso 1 calc R . .
H52C H 0.3264 0.0434 0.1700 0.029 Uiso 1 calc R . .
C53 C 0.53770(15) 0.37397(15) 0.15241(6) 0.0166(4) Uani 1 d . . .
H53A H 0.5751 0.4069 0.1315 0.020 Uiso 1 calc R . .
H53B H 0.5667 0.3917 0.1792 0.020 Uiso 1 calc R . .
C54 C 0.42120(17) 0.39664(18) 0.14965(7) 0.0264(5) Uani 1 d . . .
H54A H 0.3923 0.3780 0.1234 0.032 Uiso 1 calc R . .
H54B H 0.4122 0.4602 0.1527 0.032 Uiso 1 calc R . .
H54C H 0.3848 0.3661 0.1712 0.032 Uiso 1 calc R . .
C55 C 1.08316(16) 0.30059(16) 0.21281(6) 0.0198(4) Uani 1 d . . .
H55A H 1.0312 0.2927 0.2340 0.024 Uiso 1 calc R . .
H55B H 1.0603 0.3507 0.1957 0.024 Uiso 1 calc R . .
C56 C 1.18872(19) 0.32286(19) 0.23290(7) 0.0298(6) Uani 1 d . . .
H56A H 1.2128 0.2730 0.2494 0.036 Uiso 1 calc R . .
H56B H 1.1814 0.3747 0.2501 0.036 Uiso 1 calc R . .
H56C H 1.2395 0.3351 0.2121 0.036 Uiso 1 calc R . .
C57 C 1.02462(15) -0.02704(15) 0.19746(6) 0.0165(4) Uani 1 d . . .
H57A H 0.9885 -0.0623 0.1763 0.020 Uiso 1 calc R . .
H57B H 0.9752 -0.0167 0.2194 0.020 Uiso 1 calc R . .
C58 C 1.11928(16) -0.07865(16) 0.21429(6) 0.0194(4) Uani 1 d . . .
H58A H 1.1721 -0.0826 0.1936 0.023 Uiso 1 calc R . .
H58B H 1.0974 -0.1379 0.2219 0.023 Uiso 1 calc R . .
H58C H 1.1486 -0.0483 0.2381 0.023 Uiso 1 calc R . .
C59 C 1.17438(15) 0.14748(16) 0.08261(5) 0.0186(4) Uani 1 d . . .
H59A H 1.1633 0.2059 0.0701 0.022 Uiso 1 calc R . .
H59B H 1.1413 0.1029 0.0647 0.022 Uiso 1 calc R . .
C60 C 1.29138(17) 0.1290(2) 0.08681(7) 0.0300(6) Uani 1 d . . .
H60A H 1.3238 0.1721 0.1052 0.036 Uiso 1 calc R . .
H60B H 1.3229 0.1333 0.0603 0.036 Uiso 1 calc R . .
H60C H 1.3023 0.0697 0.0977 0.036 Uiso 1 calc R . .
S100 S 0.90273(4) 0.19601(4) 0.044170(13) 0.01421(11) Uani 1 d . . .
O101 O 0.99521(11) 0.25225(11) 0.04063(4) 0.0192(3) Uani 1 d . . .
O102 O 0.85791(12) 0.20861(11) 0.08455(4) 0.0203(3) Uani 1 d . . .
O103 O 0.82279(12) 0.21946(13) 0.01308(5) 0.0294(4) Uani 1 d . . .
O104 O 0.93175(13) 0.10257(11) 0.03837(4) 0.0240(3) Uani 1 d . . .
S200 S 0.72767(3) -0.00090(4) 0.244649(12) 0.01348(10) Uani 1 d . . .
O201 O 0.64132(11) 0.03944(11) 0.26672(4) 0.0184(3) Uani 1 d . . .
O202 O 0.68640(12) -0.07582(11) 0.21991(4) 0.0198(3) Uani 1 d . . .
O203 O 0.80828(11) -0.03409(11) 0.27334(4) 0.0212(3) Uani 1 d . . .
O204 O 0.77448(12) 0.06527(11) 0.21792(4) 0.0223(3) Uani 1 d . . .
S300 S 0.42039(4) 0.60111(4) 0.070251(16) 0.02509(13) Uani 1 d . . .
O301 O 0.30835(13) 0.56885(13) 0.05861(5) 0.0314(4) Uani 1 d . . .
O302 O 0.48568(15) 0.52421(15) 0.06668(6) 0.0386(5) Uani 1 d . . .
O303 O 0.41635(14) 0.63400(16) 0.11153(5) 0.0398(5) Uani 1 d . . .
O304 O 0.44593(15) 0.67097(14) 0.04218(6) 0.0375(5) Uani 1 d . . .
S400 S 0.16638(4) 0.67183(4) 0.164054(15) 0.02255(13) Uani 1 d . . .
O401 O 0.12176(17) 0.59920(15) 0.14117(6) 0.0441(5) Uani 1 d . . .
O402 O 0.28522(15) 0.65212(18) 0.17062(6) 0.0490(6) Uani 1 d . . .
O403 O 0.12665(16) 0.67933(15) 0.20408(5) 0.0421(5) Uani 1 d . . .
O404 O 0.15769(18) 0.75256(14) 0.14031(6) 0.0427(5) Uani 1 d . . .
OW1 O 0.81886(11) 0.06307(11) 0.13502(4) 0.0186(3) Uani 1 d D . .
H1C H 0.808(2) 0.0766(15) 0.1585(3) 0.022 Uiso 1 d D . .
H1D H 0.829(2) 0.1087(11) 0.1224(6) 0.022 Uiso 1 d D . .
OW2 O 0.97427(13) 0.48194(12) 0.16759(5) 0.0245(3) Uani 1 d D . .
H2C H 0.9481(18) 0.4942(17) 0.1893(5) 0.029 Uiso 1 d D . .
H2D H 1.0216(16) 0.5188(15) 0.1643(7) 0.029 Uiso 1 d D . .
OW3 O 0.77741(12) 0.41123(12) 0.15357(4) 0.0227(3) Uani 1 d D . .
H3C H 0.8332(14) 0.4380(19) 0.1506(8) 0.040(9) Uiso 1 d D . .
H3D H 0.7520(19) 0.4321(19) 0.1744(6) 0.038(8) Uiso 1 d D . .
OW4 O 0.18442(15) 0.70045(14) 0.05894(5) 0.0352(4) Uani 1 d D . .
H4C H 0.186(3) 0.7356(15) 0.0395(5) 0.042 Uiso 1 d D . .
H4D H 0.183(3) 0.7317(15) 0.0796(5) 0.042 Uiso 1 d D . .
OW5 O 0.80746(13) 0.28387(12) 0.22059(5) 0.0238(3) Uani 1 d D . .
H5C H 0.807(2) 0.3236(12) 0.2380(5) 0.029 Uiso 1 d D . .
H5D H 0.808(2) 0.3099(15) 0.1985(4) 0.029 Uiso 1 d D . .
OW6 O 0.39949(15) 0.37369(15) 0.01951(6) 0.0380(5) Uani 1 d D . .
H6C H 0.442(2) 0.372(2) 0.0014(7) 0.046 Uiso 1 d D . .
H6D H 0.406(2) 0.4200(13) 0.0318(8) 0.046 Uiso 1 d D . .
OW7 O 0.51212(16) 0.81502(14) 0.19814(6) 0.0358(4) Uani 1 d D . .
H7C H 0.4624(17) 0.8411(17) 0.1855(9) 0.043 Uiso 1 d D . .
H7D H 0.545(2) 0.8577(14) 0.2092(9) 0.043 Uiso 1 d D . .
OW8 O 0.23184(18) 0.94853(18) 0.02625(6) 0.0505(6) Uani 1 d D . .
H8C H 0.200(3) 0.9131(16) 0.0108(8) 0.061 Uiso 1 d D . .
H8D H 0.233(3) 0.9953(13) 0.0127(9) 0.061 Uiso 1 d D . .
OW9 O 1.39480(19) -0.15018(17) 0.06929(6) 0.0457(5) Uani 1 d D . .
H9C H 1.346(2) -0.1259(19) 0.0566(9) 0.055 Uiso 1 d D . .
H9D H 1.401(3) -0.1998(12) 0.0584(10) 0.055 Uiso 1 d D . .
OW10 O 1.34166(17) -0.13633(16) 0.14891(6) 0.0415(5) Uani 1 d D . .
H10C H 1.358(2) -0.142(2) 0.1244(3) 0.050 Uiso 1 d D . .
H10D H 1.390(2) -0.164(2) 0.1613(7) 0.050 Uiso 1 d D . .
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'
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
C2 N1 C30 109.50(14) . . ?
C2 N1 H1A 109.8 . . ?
C30 N1 H1A 109.8 . . ?
C2 N1 H1B 109.8 . . ?
C30 N1 H1B 109.8 . . ?
H1A N1 H1B 108.2 . . ?
C3 N8 C7 118.40(16) . . ?
C9 N10 C11 110.75(15) . . ?
C9 N10 H10A 109.5 . . ?
C11 N10 H10A 109.5 . . ?
C9 N10 H10B 109.5 . . ?
C11 N10 H10B 109.5 . . ?
H10A N10 H10B 108.1 . . ?
C17 N16 C15 108.89(14) . . ?
C17 N16 H16A 109.9 . . ?
C15 N16 H16A 109.9 . . ?
C17 N16 H16B 109.9 . . ?
C15 N16 H16B 109.9 . . ?
H16A N16 H16B 108.3 . . ?
C22 N23 C18 117.52(18) . . ?
C24 N25 C26 111.69(15) . . ?
C24 N25 H25A 109.3 . . ?
C26 N25 H25A 109.3 . . ?
C24 N25 H25B 109.3 . . ?
C26 N25 H25B 109.3 . . ?
H25A N25 H25B 107.9 . . ?
C36 N35 C34 112.65(16) . . ?
C36 N35 H35A 109.1 . . ?
C34 N35 H35A 109.1 . . ?
C36 N35 H35B 109.1 . . ?
C34 N35 H35B 109.1 . . ?
H35A N35 H35B 107.8 . . ?
C37 N42 C41 117.93(16) . . ?
C43 N44 C45 112.14(15) . . ?
C43 N44 H44A 109.2 . . ?
C45 N44 H44A 109.2 . . ?
C43 N44 H44B 109.2 . . ?
C45 N44 H44B 109.2 . . ?
H44A N44 H44B 107.9 . . ?
N1 C2 C3 111.49(15) . . ?
N1 C2 H2A 109.3 . . ?
C3 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N8 C3 C4 122.74(18) . . ?
N8 C3 C2 116.61(16) . . ?
C4 C3 C2 120.64(17) . . ?
C5 C4 C3 117.82(18) . . ?
C5 C4 H4 121.1 . . ?
C3 C4 H4 121.1 . . ?
C6 C5 C4 119.98(18) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C7 C6 C5 117.72(19) . . ?
C7 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
N8 C7 C6 123.30(18) . . ?
N8 C7 C9 115.01(16) . . ?
C6 C7 C9 121.69(18) . . ?
N10 C9 C7 109.51(17) . . ?
N10 C9 H9A 109.8 . . ?
C7 C9 H9A 109.8 . . ?
N10 C9 H9B 109.8 . . ?
C7 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
N10 C11 C12 109.83(15) . . ?
N10 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
N10 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C50 C12 C13 120.97(17) . . ?
C50 C12 C11 118.98(17) . . ?
C13 C12 C11 120.04(19) . . ?
C14 C13 C12 118.42(19) . . ?
C14 C13 C53 121.06(18) . . ?
C12 C13 C53 120.16(17) . . ?
C47 C14 C13 120.81(18) . . ?
C47 C14 C15 120.19(16) . . ?
C13 C14 C15 118.90(19) . . ?
N16 C15 C14 114.04(14) . . ?
N16 C15 H15A 108.7 . . ?
C14 C15 H15A 108.7 . . ?
N16 C15 H15B 108.7 . . ?
C14 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N16 C17 C18 113.98(15) . . ?
N16 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
N16 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
N23 C18 C19 122.98(18) . . ?
N23 C18 C17 117.80(18) . . ?
C19 C18 C17 119.20(17) . . ?
C20 C19 C18 118.24(18) . . ?
C20 C19 H19 120.9 . . ?
C18 C19 H19 120.9 . . ?
C21 C20 C19 119.3(2) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C20 C21 C22 118.31(19) . . ?
C20 C21 H21 120.8 . . ?
C22 C21 H21 120.8 . . ?
N23 C22 C21 123.58(18) . . ?
N23 C22 C24 117.18(18) . . ?
C21 C22 C24 119.19(18) . . ?
N25 C24 C22 111.32(16) . . ?
N25 C24 H24A 109.4 . . ?
C22 C24 H24A 109.4 . . ?
N25 C24 H24B 109.4 . . ?
C22 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
N25 C26 C27 111.55(16) . . ?
N25 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
N25 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C33 120.51(19) . . ?
C28 C27 C26 119.29(19) . . ?
C33 C27 C26 120.20(17) . . ?
C27 C28 C29 119.21(18) . . ?
C27 C28 C55 120.62(19) . . ?
C29 C28 C55 120.12(17) . . ?
C31 C29 C28 120.58(16) . . ?
C31 C29 C30 119.48(18) . . ?
C28 C29 C30 119.61(18) . . ?
N1 C30 C29 116.14(14) . . ?
N1 C30 H30A 108.3 . . ?
C29 C30 H30A 108.3 . . ?
N1 C30 H30B 108.3 . . ?
C29 C30 H30B 108.3 . . ?
H30A C30 H30B 107.4 . . ?
C29 C31 C32 119.17(18) . . ?
C29 C31 C57 120.53(16) . . ?
C32 C31 C57 120.21(18) . . ?
C33 C32 C31 120.74(18) . . ?
C33 C32 C34 119.87(16) . . ?
C31 C32 C34 119.40(18) . . ?
C32 C33 C27 119.30(17) . . ?
C32 C33 C59 120.17(18) . . ?
C27 C33 C59 120.36(19) . . ?
N35 C34 C32 109.96(16) . . ?
N35 C34 H34A 109.7 . . ?
C32 C34 H34A 109.7 . . ?
N35 C34 H34B 109.7 . . ?
C32 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
N35 C36 C37 110.87(16) . . ?
N35 C36 H36A 109.5 . . ?
C37 C36 H36A 109.5 . . ?
N35 C36 H36B 109.5 . . ?
C37 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
N42 C37 C38 122.90(18) . . ?
N42 C37 C36 115.65(16) . . ?
C38 C37 C36 121.29(18) . . ?
C39 C38 C37 118.44(18) . . ?
C39 C38 H38 120.8 . . ?
C37 C38 H38 120.8 . . ?
C38 C39 C40 119.48(18) . . ?
C38 C39 H39 120.3 . . ?
C40 C39 H39 120.3 . . ?
C41 C40 C39 118.06(19) . . ?
C41 C40 H40 121.0 . . ?
C39 C40 H40 121.0 . . ?
N42 C41 C40 123.19(18) . . ?
N42 C41 C43 114.89(16) . . ?
C40 C41 C43 121.73(18) . . ?
N44 C43 C41 111.65(17) . . ?
N44 C43 H43A 109.3 . . ?
C41 C43 H43A 109.3 . . ?
N44 C43 H43B 109.3 . . ?
C41 C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
C46 C45 N44 111.28(15) . . ?
C46 C45 H45A 109.4 . . ?
N44 C45 H45A 109.4 . . ?
C46 C45 H45B 109.4 . . ?
N44 C45 H45B 109.4 . . ?
H45A C45 H45B 108.0 . . ?
C50 C46 C47 120.5(2) . . ?
C50 C46 C45 119.93(18) . . ?
C47 C46 C45 119.58(17) . . ?
C14 C47 C46 119.30(17) . . ?
C14 C47 C48 120.74(18) . . ?
C46 C47 C48 119.88(19) . . ?
C47 C48 C49 112.96(16) . . ?
C47 C48 H48A 109.0 . . ?
C49 C48 H48A 109.0 . . ?
C47 C48 H48B 109.0 . . ?
C49 C48 H48B 109.0 . . ?
H48A C48 H48B 107.8 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C12 C50 C46 118.99(18) . . ?
C12 C50 C51 119.44(17) . . ?
C46 C50 C51 121.34(19) . . ?
C50 C51 C52 111.58(16) . . ?
C50 C51 H51A 109.3 . . ?
C52 C51 H51A 109.3 . . ?
C50 C51 H51B 109.3 . . ?
C52 C51 H51B 109.3 . . ?
H51A C51 H51B 108.0 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C13 C53 C54 110.52(18) . . ?
C13 C53 H53A 109.5 . . ?
C54 C53 H53A 109.5 . . ?
C13 C53 H53B 109.5 . . ?
C54 C53 H53B 109.5 . . ?
H53A C53 H53B 108.1 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C28 C55 C56 113.31(19) . . ?
C28 C55 H55A 108.9 . . ?
C56 C55 H55A 108.9 . . ?
C28 C55 H55B 108.9 . . ?
C56 C55 H55B 108.9 . . ?
H55A C55 H55B 107.7 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C31 C57 C58 111.28(16) . . ?
C31 C57 H57A 109.4 . . ?
C58 C57 H57A 109.4 . . ?
C31 C57 H57B 109.4 . . ?
C58 C57 H57B 109.4 . . ?
H57A C57 H57B 108.0 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C33 C59 C60 110.88(15) . . ?
C33 C59 H59A 109.5 . . ?
C60 C59 H59A 109.5 . . ?
C33 C59 H59B 109.5 . . ?
C60 C59 H59B 109.5 . . ?
H59A C59 H59B 108.1 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O101 S100 O103 110.58(9) . . ?
O101 S100 O102 109.29(9) . . ?
O103 S100 O102 108.55(10) . . ?
O101 S100 O104 109.93(10) . . ?
O103 S100 O104 108.26(10) . . ?
O102 S100 O104 110.22(9) . . ?
O203 S200 O201 110.26(8) . . ?
O203 S200 O204 109.21(9) . . ?
O201 S200 O204 109.63(10) . . ?
O203 S200 O202 108.97(9) . . ?
O201 S200 O202 109.16(9) . . ?
O204 S200 O202 109.58(9) . . ?
O302 S300 O304 113.42(12) . . ?
O302 S300 O303 112.91(12) . . ?
O304 S300 O303 111.28(13) . . ?
O302 S300 O301 104.99(12) . . ?
O304 S300 O301 107.10(11) . . ?
O303 S300 O301 106.52(10) . . ?
O403 S400 O401 113.43(13) . . ?
O403 S400 O404 113.94(13) . . ?
O401 S400 O404 109.61(13) . . ?
O403 S400 O402 104.81(11) . . ?
O401 S400 O402 107.30(14) . . ?
O404 S400 O402 107.24(14) . . ?
H1C OW1 H1D 107.6(15) . . ?
H2C OW2 H2D 106.0(15) . . ?
H3C OW3 H3D 105.5(15) . . ?
H4C OW4 H4D 105.7(15) . . ?
H5C OW5 H5D 105.1(15) . . ?
H6C OW6 H6D 109.3(17) . . ?
H7C OW7 H7D 102.4(15) . . ?
H8C OW8 H8D 103.5(15) . . ?
H9C OW9 H9D 104.8(15) . . ?
H10C OW10 H10D 102.5(15) . . ?
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
N1 C2 1.488(2) . ?
N1 C30 1.507(2) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
N8 C3 1.335(2) . ?
N8 C7 1.340(2) . ?
N10 C9 1.502(2) . ?
N10 C11 1.515(2) . ?
N10 H10A 0.9200 . ?
N10 H10B 0.9200 . ?
N16 C17 1.485(2) . ?
N16 C15 1.510(2) . ?
N16 H16A 0.9200 . ?
N16 H16B 0.9200 . ?
N23 C22 1.336(3) . ?
N23 C18 1.346(2) . ?
N25 C24 1.484(3) . ?
N25 C26 1.509(2) . ?
N25 H25A 0.9200 . ?
N25 H25B 0.9200 . ?
N35 C36 1.490(3) . ?
N35 C34 1.509(2) . ?
N35 H35A 0.9200 . ?
N35 H35B 0.9200 . ?
N42 C37 1.342(2) . ?
N42 C41 1.344(3) . ?
N44 C43 1.500(3) . ?
N44 C45 1.511(2) . ?
N44 H44A 0.9200 . ?
N44 H44B 0.9200 . ?
C2 C3 1.501(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.399(3) . ?
C4 C5 1.389(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(3) . ?
C6 H6 0.9500 . ?
C7 C9 1.506(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 C12 1.517(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C50 1.401(3) . ?
C12 C13 1.412(3) . ?
C13 C14 1.411(3) . ?
C13 C53 1.519(3) . ?
C14 C47 1.402(3) . ?
C14 C15 1.515(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C17 C18 1.507(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.398(3) . ?
C19 C20 1.390(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.384(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.392(3) . ?
C21 H21 0.9500 . ?
C22 C24 1.516(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 C27 1.513(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.406(3) . ?
C27 C33 1.408(3) . ?
C28 C29 1.408(3) . ?
C28 C55 1.514(3) . ?
C29 C31 1.402(3) . ?
C29 C30 1.518(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.408(2) . ?
C31 C57 1.520(3) . ?
C32 C33 1.400(3) . ?
C32 C34 1.517(3) . ?
C33 C59 1.521(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C36 C37 1.514(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.394(3) . ?
C38 C39 1.384(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.393(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.390(3) . ?
C40 H40 0.9500 . ?
C41 C43 1.508(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C45 C46 1.510(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C50 1.407(3) . ?
C46 C47 1.409(3) . ?
C47 C48 1.522(3) . ?
C48 C49 1.535(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.526(3) . ?
C51 C52 1.534(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.537(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.533(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C58 1.540(3) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.533(3) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
S100 O101 1.4718(16) . ?
S100 O103 1.4795(14) . ?
S100 O102 1.4835(14) . ?
S100 O104 1.4840(18) . ?
S200 O203 1.4766(14) . ?
S200 O201 1.4788(15) . ?
S200 O204 1.4796(16) . ?
S200 O202 1.4935(16) . ?
S300 O302 1.447(2) . ?
S300 O304 1.456(2) . ?
S300 O303 1.4591(17) . ?
S300 O301 1.5600(17) . ?
S400 O403 1.4386(19) . ?
S400 O401 1.450(2) . ?
S400 O404 1.462(2) . ?
S400 O402 1.566(2) . ?
OW1 H1C 0.821(9) . ?
OW1 H1D 0.824(9) . ?
OW2 H2C 0.824(9) . ?
OW2 H2D 0.837(10) . ?
OW3 H3C 0.833(10) . ?
OW3 H3D 0.833(10) . ?
OW4 H4C 0.838(10) . ?
OW4 H4D 0.835(10) . ?
OW5 H5C 0.836(10) . ?
OW5 H5D 0.832(9) . ?
OW6 H6C 0.827(10) . ?
OW6 H6D 0.816(10) . ?
OW7 H7C 0.852(10) . ?
OW7 H7D 0.855(10) . ?
OW8 H8C 0.840(10) . ?
OW8 H8D 0.842(10) . ?
OW9 H9C 0.833(10) . ?
OW9 H9D 0.842(10) . ?
OW10 H10C 0.849(10) . ?
OW10 H10D 0.844(10) . ?
