#------------------------------------------------------------------------------
#$Date: 2023-07-15 03:48:46 +0200 (Sat, 15 Jul 2023) $
#$Revision: 285221 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/28/2022822.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2022822
loop_
_publ_author_name
'Kubono, Koji'
'Tanaka, Ryoichi'
'Kashiwagi, Yukiyasu'
'Tani, Keita'
'Yokoi, Kunihiko'
_publ_section_title
;
Crystal structure of
poly[(acetonitrile-\kN)(\m3-7-{[bis(pyridin-2-ylmethyl)amino]methyl}-8-hydroxyquinoline-5-sulfonato-\k4
N,O:O′:O′′)sodium]
;
_journal_coeditor_code YZ2037
_journal_issue 8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989023005959
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '[Na (C22 H19 N4 O4 S) (C2 H3 N1)]'
_chemical_formula_moiety 'C24 H22 N5 Na O4 S'
_chemical_formula_sum 'C24 H22 N5 Na O4 S'
_chemical_formula_weight 499.52
_chemical_name_systematic
Poly[(acetonitrile-\kN)(\m~3~-7-{[bis(pyridin-2-ylmethyl)amino]methyl}-8-hydroxyquinoline-5-sulfonato-\k^4^N,O:O':O'')sodium]
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.0000
_cell_angle_beta 106.378(8)
_cell_angle_gamma 90.0000
_cell_formula_units_Z 4
_cell_length_a 10.4951(4)
_cell_length_b 14.1401(5)
_cell_length_c 16.9249(6)
_cell_measurement_reflns_used 16856
_cell_measurement_temperature 173
_cell_measurement_theta_max 27.42
_cell_measurement_theta_min 2.06
_cell_volume 2409.77(18)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2016)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare, et al., 1993)
;
_diffrn_ambient_temperature 173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0420
_diffrn_reflns_av_unetI/netI 0.0347
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 23162
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.426
_diffrn_reflns_theta_min 2.483
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.193
_exptl_absorpt_correction_T_max 0.971
_exptl_absorpt_correction_T_min 0.867
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.377
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1040.00
_exptl_crystal_size_max 0.250
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.150
_refine_diff_density_max 0.32
_refine_diff_density_min -0.30
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_hydrogen_treatment mixed
_refine_ls_number_parameters 321
_refine_ls_number_reflns 5490
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0706
_refine_ls_R_factor_gt 0.0435
_refine_ls_shift/su_max 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0403P)^2^+1.2511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0932
_refine_ls_wR_factor_ref 0.1028
_reflns_number_gt 4023
_reflns_number_total 5490
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_data_source_file yz2037sup1.cif
_cod_data_source_block I
_cod_database_code 2022822
_shelx_hkl_file
;
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-10 5 16 4.14 11.01
-10 -5 16 -2.11 12.22
-10 5 15 13.22 11.06
-10 5 15 20.51 10.98
-10 -5 15 -0.00 13.01
-10 5 14 42.92 10.50
-10 5 14 17.97 10.95
-10 -5 14 -3.10 12.42
-10 5 13 187.60 12.44
-10 5 13 177.90 13.27
-10 -5 13 163.85 15.24
-10 5 12 16.37 9.49
-10 5 12 12.48 9.84
-10 -5 12 36.03 11.75
-10 5 11 59.66 9.17
-10 5 11 35.74 10.09
-10 -5 11 56.39 19.11
-10 5 10 14.87 8.67
10 5 -10 8.97 2.23
10 5 -10 10.51 9.79
-10 5 10 6.71 8.40
-10 -5 10 15.45 11.36
10 -5 -10 11.91 3.76
10 5 -9 243.75 13.93
10 5 -9 239.02 6.03
-10 5 9 225.42 11.32
10 -5 -9 224.19 6.98
-10 -5 9 235.23 22.68
10 5 -8 92.48 5.38
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10 5 -8 104.19 11.63
10 -5 -8 89.13 5.75
-10 -5 8 108.71 12.70
10 5 -7 72.60 5.75
-10 5 7 76.93 8.87
10 5 -7 87.40 11.48
10 -5 -7 82.89 5.85
-10 -5 7 69.65 12.47
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10 5 -6 9.29 9.73
10 -5 -6 11.23 5.30
-10 -5 6 18.83 10.98
-10 5 5 5.01 6.83
10 5 -5 -0.96 10.04
10 -5 -5 17.81 5.93
-10 -5 5 24.86 11.32
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10 5 -4 130.16 12.11
10 -5 -4 106.73 7.68
-10 -5 4 115.55 19.67
-10 5 3 20.50 6.98
10 5 -3 34.90 10.62
10 -5 -3 32.62 10.91
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10 -5 -2 -1.47 7.39
10 -5 -2 -1.00 6.16
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10 -5 -1 269.94 16.78
10 -5 -1 267.03 9.91
-10 -5 1 272.90 23.12
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10 -5 0 6.98 9.27
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10 -5 0 18.14 8.22
10 5 1 12.89 10.54
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10 -5 1 5.05 5.76
-10 -5 -1 -10.80 11.40
10 -5 1 -0.16 8.60
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10 -5 2 30.34 6.53
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-10 -5 -3 173.05 14.70
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10 -5 4 44.13 6.94
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10 -5 5 53.37 10.49
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10 -5 6 -4.71 6.60
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10 -6 -10 3.63 4.38
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-10 -6 9 329.57 16.92
10 -6 -9 325.03 8.99
10 6 -8 6.69 4.46
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10 6 -8 20.24 9.29
10 -6 -8 2.30 4.81
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10 -6 -7 54.65 5.97
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10 -6 -6 -5.46 5.65
-10 -6 6 11.17 10.96
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10 -6 -5 16.66 6.21
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10 6 -4 65.82 11.33
10 -6 -4 79.50 7.72
-10 -6 4 82.55 12.84
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10 6 -3 81.66 12.11
10 -6 -3 81.96 8.28
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10 6 -2 -1.65 10.50
10 -6 -2 -5.10 7.48
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10 -6 -1 237.92 11.58
10 -6 -1 240.99 8.78
-10 -6 1 246.18 15.92
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10 -6 0 13.19 8.31
10 -6 0 -2.66 8.14
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10 -6 1 9.33 5.73
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10 -6 1 31.21 13.88
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10 -6 3 25.20 10.35
10 -6 3 -0.21 5.77
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10 -6 4 2.80 5.58
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10 -6 4 1.70 10.16
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10 -6 5 12.55 9.49
-10 -6 -5 47.13 13.29
10 -6 5 26.71 11.87
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10 -6 6 80.25 7.23
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10 -6 6 68.93 13.17
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10 7 -10 156.32 13.02
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10 -7 -9 16.91 5.40
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10 7 -8 28.05 5.24
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10 -7 -8 24.94 8.98
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10 -7 -7 -1.10 8.96
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10 -7 -6 7.36 9.67
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10 -7 -5 -3.02 6.49
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10 -7 -4 2.27 6.75
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10 -7 -3 19.73 7.79
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10 -7 -2 92.94 9.49
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10 7 -1 16.00 11.71
10 -7 -1 16.00 8.53
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10 -7 3 20.45 10.56
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10 8 -10 8.68 6.44
10 8 -10 6.26 15.92
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10 -8 -10 -2.05 8.96
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10 -8 -7 1.61 6.45
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10 -8 -6 -4.09 6.52
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10 -8 -4 -12.71 7.35
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10 -8 -3 2.53 8.15
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10 -8 -2 -3.78 13.30
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10 -8 -1 5.47 8.93
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10 -9 -10 10.30 6.52
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10 9 -9 99.29 13.14
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10 -9 -9 99.72 12.08
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10 9 -8 145.54 8.15
10 9 -8 175.45 13.76
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10 -9 -8 149.63 13.30
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10 -9 -5 -9.17 7.64
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10 -9 -4 52.40 8.75
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10 -9 -3 2.51 8.39
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10 -9 -2 4.36 9.15
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10 -9 -1 67.48 10.53
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10 -9 0 31.25 10.52
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10 -9 1 0.49 10.31
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10 -9 2 -23.10 17.22
-10 -9 -2 3.14 14.09
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10 -10 -10 6.28 7.37
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10 10 -9 4.19 10.93
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-10 -10 9 -16.66 12.22
10 -10 -9 -4.93 7.28
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10 10 -8 77.85 11.03
10 10 -8 71.56 12.69
-10 10 8 60.96 7.64
-10 -10 8 73.15 20.34
10 -10 -8 59.81 8.69
-10 10 7 20.39 6.64
10 10 -7 34.58 11.57
10 10 -7 32.60 18.03
-10 10 7 22.70 6.66
-10 -10 7 31.42 12.98
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10 10 -4 0.53 8.65
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-10 10 4 6.68 7.38
-10 -10 4 11.75 19.40
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10 10 -3 5.08 11.47
10 -10 -3 -11.53 8.91
-10 -10 3 8.52 12.47
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10 10 -2 141.06 14.14
10 -10 -2 117.65 12.29
-10 -10 2 122.86 15.48
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10 -10 -1 20.24 10.39
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10 -10 0 5.92 10.33
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-10 -10 -2 35.43 14.70
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-10 11 11 9.53 8.49
-10 11 11 6.31 8.52
-10 -11 11 16.48 12.93
-10 11 10 53.28 12.54
10 11 -10 51.56 12.30
-10 11 10 41.80 8.61
-10 -11 10 61.09 13.63
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10 11 -9 -7.22 11.28
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-10 -11 9 0.35 19.68
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-10 11 7 5.98 5.89
-10 -11 7 1.77 18.66
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10 11 -6 5.56 11.63
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-10 -11 6 4.30 12.74
10 -11 -6 27.03 8.86
10 11 -5 15.06 13.51
10 11 -5 25.43 11.56
10 -11 -5 5.64 9.38
-10 -11 5 34.90 20.01
10 11 -4 39.05 9.49
10 11 -4 50.31 12.59
10 -11 -4 29.83 10.06
-10 -11 4 36.81 13.32
10 11 -3 13.47 9.82
10 11 -3 12.04 12.78
10 -11 -3 18.21 10.22
-10 -11 3 34.57 21.01
10 11 -2 6.47 10.51
10 11 -2 6.32 12.95
10 -11 -2 16.83 16.33
-10 -11 2 2.21 13.30
10 11 -1 12.39 11.08
10 11 -1 -9.05 13.44
10 -11 -1 12.66 10.71
-10 -11 1 6.48 14.16
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10 -11 1 1.75 11.65
-10 -11 -1 0.55 14.09
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10 12 -8 49.40 12.86
10 -12 -8 22.82 9.83
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10 -12 -7 4.15 9.25
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10 12 -6 5.90 8.62
10 -12 -6 8.96 14.76
-10 -12 6 -2.12 21.01
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10 12 -5 10.39 9.40
10 -12 -5 25.14 10.16
-10 -12 5 27.70 13.72
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10 12 -4 13.82 12.59
10 -12 -4 12.12 10.28
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10 12 -3 12.17 12.96
10 -12 -3 5.08 10.80
-10 -12 3 22.91 13.80
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-12 7 5 17.82 12.46
12 7 -5 -10.42 13.04
12 -7 -5 10.64 11.98
-12 -7 5 9.30 14.35
-12 7 4 16.22 12.35
12 7 -4 12.11 13.58
12 -7 -4 20.63 8.72
-12 -7 4 8.73 14.44
-12 7 3 9.15 11.68
12 7 -3 4.54 13.14
12 -7 -3 12.28 9.21
-12 -7 3 24.80 14.85
-12 7 2 22.38 11.74
12 7 -2 -3.97 21.06
12 -7 -2 11.90 9.93
-12 -7 2 14.76 14.94
-12 7 1 4.21 11.11
12 7 -1 35.85 13.56
12 -7 -1 -11.88 9.88
-12 -7 1 2.07 14.85
12 7 0 57.63 15.11
-12 7 0 42.47 12.16
12 -7 0 61.28 11.69
-12 -7 0 70.34 24.40
12 8 -9 92.75 14.29
-12 8 9 88.87 15.54
-12 8 9 62.70 10.45
-12 -8 9 72.63 16.41
-12 8 8 34.91 9.17
12 8 -8 17.47 14.11
-12 8 8 37.45 9.26
-12 -8 8 53.83 23.68
12 -8 -8 24.82 11.63
12 8 -7 95.22 8.65
-12 8 7 103.79 10.13
12 8 -7 138.62 15.22
-12 8 7 100.38 10.17
-12 -8 7 135.51 17.45
12 -8 -7 86.76 13.88
12 8 -6 5.60 7.72
-12 8 6 1.30 7.79
12 8 -6 11.09 13.14
-12 8 6 4.17 7.71
-12 -8 6 31.89 22.24
12 -8 -6 -0.29 7.86
12 8 -5 8.77 8.69
-12 8 5 -5.51 7.29
12 8 -5 -4.09 13.00
12 -8 -5 -1.98 7.87
-12 -8 5 13.07 14.15
-12 8 4 -1.56 7.19
12 8 -4 -4.32 13.54
12 -8 -4 -8.84 13.34
-12 -8 4 13.55 22.38
-12 8 3 74.76 8.56
12 8 -3 90.40 15.81
12 -8 -3 92.62 11.38
-12 -8 3 91.20 17.11
-12 8 2 1.14 6.50
12 8 -2 9.96 13.78
12 -8 -2 -12.37 15.22
-12 -8 2 -10.47 14.90
-13 0 12 39.29 13.79
-13 0 11 -3.60 13.27
-13 0 10 16.63 12.82
-13 0 9 16.17 12.28
-13 0 8 -24.56 12.49
13 0 -7 -16.36 10.42
-13 0 7 -8.95 12.17
13 0 -6 -17.03 16.82
-13 0 6 39.07 12.37
13 0 -5 22.44 10.56
-13 0 5 -4.44 18.58
13 0 -4 55.92 17.43
-13 0 4 21.99 12.52
13 0 -3 1.82 10.69
-13 0 3 3.57 11.60
13 0 -2 13.33 16.16
-13 0 2 -9.32 18.33
13 0 -1 0.59 10.53
-13 0 1 4.11 11.55
13 0 0 3.34 16.86
-13 0 0 -16.24 12.04
-13 1 11 13.67 12.33
-13 -1 11 28.87 21.21
-13 1 10 -6.94 18.54
-13 -1 10 1.93 12.70
-13 1 9 29.94 12.74
-13 -1 9 7.86 20.20
13 1 -8 1.92 11.21
-13 1 8 18.38 18.39
-13 -1 8 3.50 12.54
13 1 -7 81.65 18.98
-13 1 7 59.53 13.42
13 -1 -7 78.60 11.65
-13 -1 7 79.31 21.25
13 1 -6 9.45 10.83
-13 1 6 -4.18 11.42
13 -1 -6 16.70 10.12
-13 -1 6 -27.68 12.27
13 -1 -6 0.93 9.46
13 1 -5 13.99 17.22
-13 1 5 14.29 11.61
13 -1 -5 10.14 6.75
13 -1 -5 8.27 10.17
-13 -1 5 8.78 12.18
13 1 -4 31.10 11.56
-13 1 4 16.31 11.77
13 -1 -4 34.04 10.62
-13 -1 4 22.63 12.52
13 1 -3 56.47 18.44
-13 1 3 46.43 11.77
13 -1 -3 37.05 11.19
-13 -1 3 36.76 13.28
-13 1 2 16.40 18.04
13 1 -2 -2.73 11.38
13 -1 -2 0.26 10.21
-13 -1 2 26.26 12.54
13 1 -1 51.47 12.25
-13 1 1 72.01 12.86
13 -1 -1 62.53 17.38
-13 -1 1 50.38 14.02
13 1 0 11.50 11.85
-13 1 0 25.12 12.11
13 -1 0 21.91 10.38
-13 -1 0 5.66 13.10
-13 2 11 -3.55 12.03
-13 -2 11 -2.62 13.91
-13 2 10 19.52 11.92
-13 -2 10 33.63 14.05
13 2 -9 62.26 13.59
-13 2 9 79.38 13.20
-13 -2 9 78.42 15.22
13 2 -8 25.64 12.58
-13 2 8 64.42 18.31
-13 -2 8 29.94 14.08
13 2 -7 -11.51 11.43
-13 2 7 -13.01 11.34
-13 -2 7 14.67 12.92
13 2 -6 95.97 13.38
-13 2 6 124.52 13.14
13 -2 -6 114.49 12.00
-13 -2 6 85.85 15.42
13 -2 -6 89.16 7.88
13 2 -5 12.56 12.38
-13 2 5 39.76 11.16
13 -2 -5 31.46 11.21
13 -2 -5 25.26 10.28
-13 -2 5 23.20 13.50
13 2 -4 92.37 13.91
-13 2 4 86.71 12.76
13 -2 -4 94.06 11.60
-13 -2 4 120.44 22.44
13 -2 -4 101.49 9.07
13 2 -3 13.74 12.54
-13 2 3 23.32 11.52
13 -2 -3 28.99 10.27
-13 -2 3 40.72 13.48
-13 2 2 61.35 18.46
13 2 -2 48.86 12.89
13 -2 -2 64.52 11.27
-13 -2 2 81.47 14.22
13 2 -1 19.78 11.72
-13 2 1 12.24 11.32
13 -2 -1 13.58 10.14
-13 -2 1 24.62 13.30
-13 3 11 14.48 11.65
-13 -3 11 -9.12 14.04
-13 3 10 -12.76 11.72
-13 -3 10 20.56 21.10
13 3 -9 20.49 12.64
-13 3 9 23.97 11.87
-13 -3 9 23.32 14.22
13 3 -8 26.56 19.15
-13 3 8 18.02 11.44
-13 -3 8 -11.69 21.54
-13 3 7 22.05 10.53
13 3 -7 3.72 11.68
13 -3 -7 2.20 5.62
-13 -3 7 3.52 13.67
-13 3 6 9.52 16.42
13 3 -6 -24.56 12.04
13 -3 -6 0.25 6.57
-13 -3 6 -15.49 20.45
-13 3 5 21.72 11.11
13 3 -5 13.18 12.66
13 -3 -5 23.10 11.32
-13 -3 5 22.36 13.83
13 3 -4 32.09 19.46
-13 3 4 14.79 11.09
13 -3 -4 21.92 8.35
13 -3 -4 28.16 9.74
-13 -3 4 17.01 14.21
13 3 -3 49.64 13.38
-13 3 3 52.89 11.42
13 -3 -3 52.97 15.69
-13 -3 3 58.07 14.70
13 -3 -3 41.59 9.58
13 3 -2 7.38 18.19
-13 3 2 -0.19 15.74
13 -3 -2 2.30 9.05
13 -3 -2 1.84 9.17
-13 -3 2 7.68 13.80
13 3 -1 -4.79 12.26
-13 3 1 -12.21 10.48
13 -3 -1 5.00 14.81
-13 -3 1 -29.35 21.16
13 4 -10 18.33 12.62
-13 4 10 2.46 11.51
-13 -4 10 -8.45 14.59
13 4 -9 5.88 12.67
-13 4 9 19.74 11.20
-13 -4 9 17.57 14.30
13 4 -8 14.60 12.95
-13 4 8 25.94 10.62
-13 -4 8 23.29 14.23
-13 4 7 22.18 10.47
13 4 -7 11.66 12.49
13 -4 -7 1.03 5.85
-13 -4 7 -0.46 13.48
-13 4 6 -0.61 15.65
13 4 -6 6.64 12.57
13 -4 -6 7.13 6.72
-13 -4 6 -14.62 14.15
-13 4 5 213.66 13.72
13 4 -5 193.57 16.22
13 -4 -5 175.66 10.54
-13 -4 5 175.46 18.14
-13 4 4 23.55 10.63
13 4 -4 5.28 12.76
13 -4 -4 17.92 8.39
-13 -4 4 18.53 14.39
13 4 -3 18.93 12.69
-13 4 3 9.74 9.88
13 -4 -3 9.44 9.32
-13 -4 3 40.99 21.83
13 -4 -3 5.27 8.89
13 4 -2 46.68 13.85
-13 4 2 50.74 16.47
13 -4 -2 36.28 9.66
-13 -4 2 31.32 15.05
13 -4 -2 32.66 10.01
13 5 -8 -12.39 12.72
-13 5 8 5.56 10.01
-13 -5 8 -4.53 14.30
-13 5 7 8.69 10.18
13 5 -7 15.03 19.94
13 -5 -7 12.06 9.99
-13 -5 7 4.32 22.66
-13 5 6 32.48 15.88
13 5 -6 22.30 13.61
13 -5 -6 11.66 7.34
-13 -5 6 23.12 14.94
13 5 -5 -13.58 20.54
-13 5 5 -3.79 9.53
-13 -5 5 -19.01 22.17
-13 5 4 60.30 10.71
13 5 -4 31.25 14.64
13 -5 -4 69.35 14.48
-13 -5 4 65.13 15.64
;
_shelx_hkl_checksum 22515
_shelx_res_file
;
TITL 210602pm_Na(HSO3qdpa)
shelxl.res
created by SHELXL-2018/3 at 11:19:02 on 02-Jul-2023
CELL 0.71075 10.49509 14.14011 16.92494 90.000 106.378 90.000
ZERR 4 0.00039 0.00047 0.00063 0.000 0.007 0.000
LATT 1
SYMM -X, 1/2+Y, 1/2-Z
SFAC C H N NA O S
UNIT 96 88 20 4 16 4
OMIT 1 0 0
OMIT 0 1 1
OMIT 4 2 1
L.S. 10
FMAP 2
PLAN -10
WPDB -2
BOND $H
CONF
LIST 4
TEMP -100.0
ACTA
SIZE 0.200 0.150 0.250
REM HTAB
HTAB
WGHT 0.040400 1.249300
FVAR 0.62933
S1 6 1.181144 0.466350 0.909114 11.00000 0.03110 0.03460 =
0.02578 -0.00541 0.00925 -0.00365
NA2 4 1.070431 0.101720 0.582075 11.00000 0.04138 0.03249 =
0.02816 -0.00187 0.01433 -0.00023
O3 5 1.021417 0.269041 0.585066 11.00000 0.04141 0.03066 =
0.02180 0.00007 0.00581 0.00433
O4 5 1.122788 0.559938 0.893386 11.00000 0.04236 0.03704 =
0.03750 -0.00934 0.00930 0.00377
O5 5 1.124325 0.409824 0.962842 11.00000 0.05433 0.05495 =
0.02851 -0.00505 0.01904 -0.01446
O6 5 1.324830 0.467525 0.934670 11.00000 0.03236 0.04161 =
0.04124 -0.00661 0.00476 -0.00344
N7 3 1.186868 0.181414 0.712203 11.00000 0.04045 0.02570 =
0.02819 0.00097 0.00946 0.00112
N8 3 0.788520 0.405120 0.566628 11.00000 0.03040 0.03442 =
0.02322 0.00024 0.00881 0.00144
N9 3 0.859654 0.327395 0.438310 11.00000 0.03886 0.04180 =
0.02930 -0.00028 0.01119 0.00138
N10 3 0.490050 0.362416 0.625574 11.00000 0.04018 0.05383 =
0.05492 0.00098 0.02549 0.00309
N11 3 1.222854 -0.032748 0.636194 11.00000 0.06932 0.04586 =
0.05775 -0.00145 0.01518 0.01521
C12 1 1.053168 0.316471 0.657484 11.00000 0.02897 0.02786 =
0.02382 -0.00033 0.01120 -0.00442
C13 1 1.007382 0.406338 0.667450 11.00000 0.02653 0.02869 =
0.02662 0.00215 0.00934 -0.00225
C14 1 1.047966 0.449255 0.745810 11.00000 0.02846 0.02646 =
0.02848 -0.00056 0.01117 -0.00057
AFIX 43
H14 2 1.014363 0.510196 0.752534 11.00000 -1.20000
AFIX 0
C15 1 1.133633 0.406834 0.812494 11.00000 0.02644 0.03026 =
0.02552 -0.00354 0.01061 -0.00386
C16 1 1.183400 0.314718 0.803652 11.00000 0.02814 0.02976 =
0.02583 0.00197 0.00955 -0.00464
C17 1 1.273211 0.264401 0.868801 11.00000 0.04112 0.03460 =
0.02579 0.00011 0.00440 -0.00368
AFIX 43
H17 2 1.301928 0.291025 0.922443 11.00000 -1.20000
AFIX 0
C18 1 1.317412 0.178100 0.853594 11.00000 0.04968 0.03234 =
0.03540 0.00537 -0.00261 0.00483
AFIX 43
H18 2 1.378379 0.144070 0.896296 11.00000 -1.20000
AFIX 0
C19 1 1.272220 0.139451 0.774092 11.00000 0.04895 0.02806 =
0.03613 0.00245 0.00662 0.00640
AFIX 43
H19 2 1.305452 0.079314 0.764561 11.00000 -1.20000
AFIX 0
C20 1 1.142546 0.269540 0.726096 11.00000 0.02944 0.02610 =
0.02488 0.00192 0.01146 -0.00234
C21 1 0.914299 0.456610 0.595847 11.00000 0.03370 0.02918 =
0.02815 0.00273 0.00897 -0.00019
AFIX 23
H21A 2 0.896845 0.521199 0.612841 11.00000 -1.20000
H21B 2 0.956231 0.462263 0.550483 11.00000 -1.20000
AFIX 0
C22 1 0.712994 0.434929 0.484900 11.00000 0.03670 0.04121 =
0.02947 0.00249 0.00611 0.00615
AFIX 23
H22A 2 0.716550 0.504736 0.481568 11.00000 -1.20000
H22B 2 0.618938 0.416526 0.475797 11.00000 -1.20000
AFIX 0
C23 1 0.763626 0.392485 0.417276 11.00000 0.03427 0.03396 =
0.02749 0.00103 0.00651 -0.00408
C24 1 0.707233 0.420289 0.336160 11.00000 0.04525 0.04351 =
0.03056 0.00355 0.00531 -0.00255
AFIX 43
H24 2 0.640408 0.467689 0.323134 11.00000 -1.20000
AFIX 0
C25 1 0.750289 0.377614 0.274776 11.00000 0.05755 0.06060 =
0.02559 0.00114 0.00789 -0.01314
AFIX 43
H25 2 0.713422 0.395451 0.218858 11.00000 -1.20000
AFIX 0
C26 1 0.847348 0.308858 0.295564 11.00000 0.05330 0.06076 =
0.03275 -0.01001 0.01913 -0.00847
AFIX 43
H26 2 0.877040 0.277717 0.254261 11.00000 -1.20000
AFIX 0
C27 1 0.900366 0.286295 0.377641 11.00000 0.04485 0.05141 =
0.03714 -0.00651 0.01527 -0.00034
AFIX 43
H27 2 0.968416 0.239856 0.392049 11.00000 -1.20000
AFIX 0
C28 1 0.709205 0.411155 0.624889 11.00000 0.03575 0.03493 =
0.03054 -0.00356 0.01334 0.00311
AFIX 23
H28A 2 0.666499 0.474147 0.619956 11.00000 -1.20000
H28B 2 0.768646 0.405127 0.681603 11.00000 -1.20000
AFIX 0
C29 1 0.603707 0.336081 0.610953 11.00000 0.03120 0.03974 =
0.02328 0.00293 0.00808 0.00249
C30 1 0.624978 0.245340 0.586102 11.00000 0.03571 0.03868 =
0.03717 -0.00097 0.00869 0.00256
AFIX 43
H30 2 0.706913 0.229419 0.575984 11.00000 -1.20000
AFIX 0
C31 1 0.525552 0.178189 0.576192 11.00000 0.05067 0.04260 =
0.03500 0.00125 0.00207 -0.00690
AFIX 43
H31 2 0.537800 0.115726 0.558990 11.00000 -1.20000
AFIX 0
C32 1 0.408980 0.204049 0.591812 11.00000 0.04619 0.06414 =
0.04536 0.00536 0.01115 -0.01892
AFIX 43
H32 2 0.338984 0.159710 0.586228 11.00000 -1.20000
AFIX 0
C33 1 0.395848 0.295204 0.615626 11.00000 0.03845 0.07414 =
0.07224 0.00413 0.02855 -0.00559
AFIX 43
H33 2 0.314422 0.312303 0.625879 11.00000 -1.20000
AFIX 0
C34 1 1.311231 -0.078244 0.636050 11.00000 0.06177 0.04192 =
0.04055 0.00034 0.01791 0.00185
C35 1 1.425904 -0.136876 0.636744 11.00000 0.07373 0.08676 =
0.09201 -0.00274 0.04063 0.02355
AFIX 137
H35A 2 1.481852 -0.103827 0.608024 11.00000 -1.50000
H35B 2 1.395569 -0.196938 0.608878 11.00000 -1.50000
H35C 2 1.477330 -0.149253 0.693795 11.00000 -1.50000
AFIX 0
H3 2 0.957680 0.294921 0.545686 11.00000 0.05071
HKLF 4
REM 210602pm_Na(HSO3qdpa)
REM wR2 = 0.1028, GooF = S = 1.014, Restrained GooF = 1.014 for all data
REM R1 = 0.0435 for 4023 Fo > 4sig(Fo) and 0.0706 for all 5490 data
REM 321 parameters refined using 0 restraints
END
WGHT 0.0403 1.2521
REM Instructions for potential hydrogen bonds
HTAB C19 N11
EQIV $6 -x+3, y-1/2, -z+3/2
HTAB C35 O6_$6
HTAB O3 N8
HTAB O3 N9
REM Highest difference peak 0.320, deepest hole -0.305, 1-sigma level 0.044
Q1 1 1.1583 0.4327 0.8532 11.00000 0.05 0.32
Q2 1 0.7415 0.4206 0.4490 11.00000 0.05 0.27
Q3 1 1.1088 0.2933 0.6907 11.00000 0.05 0.27
Q4 1 1.1846 0.3000 0.7617 11.00000 0.05 0.26
Q5 1 1.0138 0.4200 0.7092 11.00000 0.05 0.24
Q6 1 1.2407 0.2977 0.8306 11.00000 0.05 0.23
Q7 1 1.0243 0.3618 0.6674 11.00000 0.05 0.22
Q8 1 0.9656 0.4253 0.6361 11.00000 0.05 0.22
Q9 1 1.1790 0.3669 0.8092 11.00000 0.05 0.22
Q10 1 1.0562 0.3763 0.6607 11.00000 0.05 0.22
;
_shelx_res_checksum 6577
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S1 1.18114(5) 0.46635(3) 0.90911(3) 0.03024(12) Uani d 1 . .
Na Na2 1.07043(8) 0.10172(5) 0.58208(5) 0.03309(19) Uani d 1 . .
O O3 1.02142(14) 0.26904(9) 0.58507(8) 0.0319(3) Uani d 1 . .
O O4 1.12279(14) 0.55994(10) 0.89339(9) 0.0394(3) Uani d 1 . .
O O5 1.12432(16) 0.40982(11) 0.96284(9) 0.0444(4) Uani d 1 . .
O O6 1.32483(13) 0.46752(10) 0.93467(9) 0.0395(3) Uani d 1 . .
N N7 1.18687(17) 0.18141(11) 0.71220(10) 0.0315(4) Uani d 1 . .
N N8 0.78852(16) 0.40512(11) 0.56663(9) 0.0291(3) Uani d 1 . .
N N9 0.85965(17) 0.32740(12) 0.43831(10) 0.0363(4) Uani d 1 . .
N N10 0.49005(19) 0.36242(14) 0.62557(13) 0.0472(5) Uani d 1 . .
N N11 1.2229(2) -0.03275(15) 0.63619(14) 0.0582(6) Uani d 1 . .
C C12 1.05317(18) 0.31647(13) 0.65748(11) 0.0261(4) Uani d 1 . .
C C13 1.00738(18) 0.40634(12) 0.66745(11) 0.0269(4) Uani d 1 . .
C C14 1.04797(18) 0.44926(13) 0.74581(11) 0.0272(4) Uani d 1 . .
H H14 1.014363 0.510196 0.752534 0.033 Uiso calc 1 . .
C C15 1.13363(18) 0.40683(13) 0.81249(11) 0.0267(4) Uani d 1 . .
C C16 1.18340(18) 0.31472(13) 0.80365(11) 0.0275(4) Uani d 1 . .
C C17 1.2732(2) 0.26440(14) 0.86880(12) 0.0349(5) Uani d 1 . .
H H17 1.301928 0.291025 0.922443 0.042 Uiso calc 1 . .
C C18 1.3174(2) 0.17810(15) 0.85359(13) 0.0421(5) Uani d 1 . .
H H18 1.378379 0.144070 0.896296 0.051 Uiso calc 1 . .
C C19 1.2722(2) 0.13945(14) 0.77409(13) 0.0388(5) Uani d 1 . .
H H19 1.305452 0.079314 0.764561 0.047 Uiso calc 1 . .
C C20 1.14255(18) 0.26954(12) 0.72610(11) 0.0260(4) Uani d 1 . .
C C21 0.91430(19) 0.45661(13) 0.59585(12) 0.0303(4) Uani d 1 . .
H H21A 0.896845 0.521199 0.612841 0.036 Uiso calc 1 . .
H H21B 0.956231 0.462263 0.550483 0.036 Uiso calc 1 . .
C C22 0.7130(2) 0.43493(15) 0.48490(12) 0.0364(5) Uani d 1 . .
H H22A 0.716550 0.504736 0.481568 0.044 Uiso calc 1 . .
H H22B 0.618938 0.416526 0.475797 0.044 Uiso calc 1 . .
C C23 0.7636(2) 0.39248(14) 0.41728(12) 0.0324(4) Uani d 1 . .
C C24 0.7072(2) 0.42029(16) 0.33616(13) 0.0409(5) Uani d 1 . .
H H24 0.640408 0.467689 0.323134 0.049 Uiso calc 1 . .
C C25 0.7503(2) 0.37761(18) 0.27478(13) 0.0487(6) Uani d 1 . .
H H25 0.713422 0.395451 0.218858 0.058 Uiso calc 1 . .
C C26 0.8473(2) 0.30886(17) 0.29556(14) 0.0475(6) Uani d 1 . .
H H26 0.877040 0.277717 0.254261 0.057 Uiso calc 1 . .
C C27 0.9004(2) 0.28629(17) 0.37764(14) 0.0437(5) Uani d 1 . .
H H27 0.968416 0.239856 0.392049 0.052 Uiso calc 1 . .
C C28 0.7092(2) 0.41116(14) 0.62489(12) 0.0329(4) Uani d 1 . .
H H28A 0.666499 0.474147 0.619956 0.040 Uiso calc 1 . .
H H28B 0.768646 0.405127 0.681603 0.040 Uiso calc 1 . .
C C29 0.60371(19) 0.33608(14) 0.61095(12) 0.0313(4) Uani d 1 . .
C C30 0.6250(2) 0.24534(14) 0.58610(13) 0.0375(5) Uani d 1 . .
H H30 0.706913 0.229419 0.575984 0.045 Uiso calc 1 . .
C C31 0.5256(2) 0.17819(16) 0.57619(13) 0.0448(5) Uani d 1 . .
H H31 0.537800 0.115726 0.558990 0.054 Uiso calc 1 . .
C C32 0.4090(2) 0.20405(19) 0.59181(15) 0.0523(6) Uani d 1 . .
H H32 0.338984 0.159710 0.586228 0.063 Uiso calc 1 . .
C C33 0.3958(2) 0.2952(2) 0.61563(18) 0.0590(7) Uani d 1 . .
H H33 0.314422 0.312303 0.625879 0.071 Uiso calc 1 . .
C C34 1.3112(3) -0.07824(16) 0.63605(14) 0.0474(6) Uani d 1 . .
C C35 1.4259(3) -0.1369(2) 0.6367(2) 0.0806(10) Uani d 1 . .
H H35A 1.481852 -0.103827 0.608024 0.121 Uiso calc 1 . .
H H35B 1.395569 -0.196938 0.608878 0.121 Uiso calc 1 . .
H H35C 1.477330 -0.149253 0.693795 0.121 Uiso calc 1 . .
H H3 0.958(2) 0.2949(17) 0.5457(16) 0.051(7) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
S1 0.0311(2) 0.0346(3) 0.0258(2) -0.0037(2) 0.00925(19) -0.00541(19)
Na2 0.0414(4) 0.0325(4) 0.0282(4) -0.0002(3) 0.0143(3) -0.0019(3)
O3 0.0414(8) 0.0307(7) 0.0218(7) 0.0043(6) 0.0058(6) 0.0001(5)
O4 0.0424(8) 0.0370(8) 0.0375(8) 0.0038(6) 0.0093(7) -0.0093(6)
O5 0.0543(10) 0.0549(9) 0.0285(8) -0.0145(8) 0.0190(7) -0.0051(6)
O6 0.0324(7) 0.0416(8) 0.0412(8) -0.0034(6) 0.0048(6) -0.0066(7)
N7 0.0405(9) 0.0257(8) 0.0282(9) 0.0011(7) 0.0095(7) 0.0010(6)
N8 0.0304(8) 0.0344(8) 0.0232(8) 0.0014(7) 0.0088(7) 0.0002(6)
N9 0.0389(10) 0.0418(10) 0.0293(9) 0.0014(8) 0.0112(8) -0.0003(7)
N10 0.0402(10) 0.0538(12) 0.0549(12) 0.0031(9) 0.0255(9) 0.0010(9)
N11 0.0693(15) 0.0459(12) 0.0577(14) 0.0152(11) 0.0152(11) -0.0014(10)
C12 0.0290(9) 0.0279(9) 0.0238(9) -0.0044(7) 0.0112(8) -0.0003(7)
C13 0.0265(9) 0.0287(9) 0.0266(9) -0.0023(7) 0.0093(8) 0.0021(7)
C14 0.0285(9) 0.0265(9) 0.0285(9) -0.0006(7) 0.0112(8) -0.0006(7)
C15 0.0264(9) 0.0303(9) 0.0255(9) -0.0039(7) 0.0106(8) -0.0035(7)
C16 0.0281(9) 0.0298(9) 0.0258(9) -0.0046(8) 0.0096(8) 0.0020(7)
C17 0.0411(12) 0.0346(11) 0.0258(10) -0.0037(9) 0.0044(9) 0.0001(8)
C18 0.0497(13) 0.0323(11) 0.0354(12) 0.0048(10) -0.0026(10) 0.0054(9)
C19 0.0490(13) 0.0281(10) 0.0361(11) 0.0064(9) 0.0066(10) 0.0025(8)
C20 0.0294(9) 0.0261(9) 0.0249(9) -0.0023(7) 0.0115(8) 0.0019(7)
C21 0.0337(10) 0.0292(10) 0.0281(10) -0.0002(8) 0.0090(8) 0.0027(8)
C22 0.0367(11) 0.0412(11) 0.0295(11) 0.0061(9) 0.0061(9) 0.0025(9)
C23 0.0343(11) 0.0340(10) 0.0275(10) -0.0041(9) 0.0065(8) 0.0010(8)
C24 0.0452(12) 0.0435(12) 0.0306(11) -0.0026(10) 0.0053(9) 0.0036(9)
C25 0.0575(15) 0.0606(15) 0.0256(11) -0.0131(12) 0.0079(10) 0.0011(10)
C26 0.0533(14) 0.0608(15) 0.0327(12) -0.0085(12) 0.0191(11) -0.0100(10)
C27 0.0448(13) 0.0514(13) 0.0371(12) -0.0003(11) 0.0153(10) -0.0065(10)
C28 0.0358(11) 0.0349(11) 0.0305(10) 0.0031(8) 0.0133(9) -0.0036(8)
C29 0.0312(10) 0.0397(11) 0.0233(9) 0.0025(8) 0.0081(8) 0.0029(8)
C30 0.0357(11) 0.0387(11) 0.0372(12) 0.0026(9) 0.0087(9) -0.0010(9)
C31 0.0507(14) 0.0426(12) 0.0350(12) -0.0069(10) 0.0021(10) 0.0012(9)
C32 0.0462(14) 0.0641(16) 0.0454(14) -0.0189(12) 0.0112(11) 0.0054(12)
C33 0.0385(13) 0.0741(19) 0.0722(19) -0.0056(13) 0.0286(13) 0.0041(15)
C34 0.0618(16) 0.0419(13) 0.0405(13) 0.0019(12) 0.0179(12) 0.0003(10)
C35 0.074(2) 0.087(2) 0.092(2) 0.0236(18) 0.0406(19) -0.0027(19)
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Na Na 0.0362 0.0249
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.1246 0.1234
;
International Tables for Crystallography
(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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O6 S1 O4 . . 113.25(9) ?
O6 S1 O5 . . 113.25(9) ?
O4 S1 O5 . . 112.87(9) ?
O6 S1 C15 . . 106.16(9) ?
O4 S1 C15 . . 105.55(9) ?
O5 S1 C15 . . 104.82(9) ?
O6 S1 Na2 . 2_756 139.46(6) ?
O4 S1 Na2 . 2_756 34.63(6) ?
O5 S1 Na2 . 2_756 79.43(7) ?
C15 S1 Na2 . 2_756 107.18(6) ?
O5 Na2 O4 4_565 2_746 127.68(7) ?
O5 Na2 O3 4_565 . 101.42(6) ?
O4 Na2 O3 2_746 . 92.56(6) ?
O5 Na2 N7 4_565 . 130.30(7) ?
O4 Na2 N7 2_746 . 101.50(6) ?
O3 Na2 N7 . . 65.83(5) ?
O5 Na2 N11 4_565 . 88.66(7) ?
O4 Na2 N11 2_746 . 104.46(7) ?
O3 Na2 N11 . . 148.91(7) ?
N7 Na2 N11 . . 85.14(7) ?
O5 Na2 S1 4_565 2_746 113.91(5) ?
O4 Na2 S1 2_746 2_746 21.39(4) ?
O3 Na2 S1 . 2_746 112.83(4) ?
N7 Na2 S1 . 2_746 115.19(5) ?
N11 Na2 S1 . 2_746 88.83(6) ?
O5 Na2 Na2 4_565 3_756 57.30(5) ?
O4 Na2 Na2 2_746 3_756 76.32(5) ?
O3 Na2 Na2 . 3_756 132.85(5) ?
N7 Na2 Na2 . 3_756 160.89(5) ?
N11 Na2 Na2 . 3_756 77.20(6) ?
S1 Na2 Na2 2_746 3_756 57.86(2) ?
C12 O3 Na2 . . 120.18(11) ?
C12 O3 H3 . . 114.9(16) ?
Na2 O3 H3 . . 120.7(16) ?
S1 O4 Na2 . 2_756 123.98(9) ?
S1 O5 Na2 . 4_566 148.14(10) ?
C19 N7 C20 . . 117.48(17) ?
C19 N7 Na2 . . 124.08(13) ?
C20 N7 Na2 . . 117.42(12) ?
C22 N8 C28 . . 111.39(16) ?
C22 N8 C21 . . 112.06(15) ?
C28 N8 C21 . . 111.93(15) ?
C23 N9 C27 . . 118.06(18) ?
C29 N10 C33 . . 116.2(2) ?
C34 N11 Na2 . . 151.4(2) ?
O3 C12 C13 . . 124.01(17) ?
O3 C12 C20 . . 116.23(16) ?
C13 C12 C20 . . 119.75(17) ?
C12 C13 C14 . . 119.07(17) ?
C12 C13 C21 . . 120.28(17) ?
C14 C13 C21 . . 120.64(16) ?
C15 C14 C13 . . 122.77(17) ?
C15 C14 H14 . . 118.6 ?
C13 C14 H14 . . 118.6 ?
C14 C15 C16 . . 119.26(17) ?
C14 C15 S1 . . 119.96(14) ?
C16 C15 S1 . . 120.78(14) ?
C20 C16 C17 . . 117.06(17) ?
C20 C16 C15 . . 119.07(17) ?
C17 C16 C15 . . 123.87(17) ?
C18 C17 C16 . . 119.36(19) ?
C18 C17 H17 . . 120.3 ?
C16 C17 H17 . . 120.3 ?
C17 C18 C19 . . 119.39(19) ?
C17 C18 H18 . . 120.3 ?
C19 C18 H18 . . 120.3 ?
N7 C19 C18 . . 123.96(19) ?
N7 C19 H19 . . 118.0 ?
C18 C19 H19 . . 118.0 ?
N7 C20 C16 . . 122.71(17) ?
N7 C20 C12 . . 117.21(16) ?
C16 C20 C12 . . 120.07(16) ?
N8 C21 C13 . . 110.84(15) ?
N8 C21 H21A . . 109.5 ?
C13 C21 H21A . . 109.5 ?
N8 C21 H21B . . 109.5 ?
C13 C21 H21B . . 109.5 ?
H21A C21 H21B . . 108.1 ?
N8 C22 C23 . . 113.07(16) ?
N8 C22 H22A . . 109.0 ?
C23 C22 H22A . . 109.0 ?
N8 C22 H22B . . 109.0 ?
C23 C22 H22B . . 109.0 ?
H22A C22 H22B . . 107.8 ?
N9 C23 C24 . . 122.47(19) ?
N9 C23 C22 . . 118.05(17) ?
C24 C23 C22 . . 119.46(19) ?
C25 C24 C23 . . 118.7(2) ?
C25 C24 H24 . . 120.6 ?
C23 C24 H24 . . 120.6 ?
C26 C25 C24 . . 119.3(2) ?
C26 C25 H25 . . 120.3 ?
C24 C25 H25 . . 120.3 ?
C25 C26 C27 . . 118.6(2) ?
C25 C26 H26 . . 120.7 ?
C27 C26 H26 . . 120.7 ?
N9 C27 C26 . . 122.8(2) ?
N9 C27 H27 . . 118.6 ?
C26 C27 H27 . . 118.6 ?
N8 C28 C29 . . 112.78(16) ?
N8 C28 H28A . . 109.0 ?
C29 C28 H28A . . 109.0 ?
N8 C28 H28B . . 109.0 ?
C29 C28 H28B . . 109.0 ?
H28A C28 H28B . . 107.8 ?
N10 C29 C30 . . 122.79(19) ?
N10 C29 C28 . . 115.47(18) ?
C30 C29 C28 . . 121.73(18) ?
C31 C30 C29 . . 119.4(2) ?
C31 C30 H30 . . 120.3 ?
C29 C30 H30 . . 120.3 ?
C32 C31 C30 . . 118.4(2) ?
C32 C31 H31 . . 120.8 ?
C30 C31 H31 . . 120.8 ?
C33 C32 C31 . . 118.5(2) ?
C33 C32 H32 . . 120.8 ?
C31 C32 H32 . . 120.8 ?
N10 C33 C32 . . 124.7(2) ?
N10 C33 H33 . . 117.6 ?
C32 C33 H33 . . 117.6 ?
N11 C34 C35 . . 179.4(3) ?
C34 C35 H35A . . 109.5 ?
C34 C35 H35B . . 109.5 ?
H35A C35 H35B . . 109.5 ?
C34 C35 H35C . . 109.5 ?
H35A C35 H35C . . 109.5 ?
H35B C35 H35C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
S1 O6 . 1.4469(14) ?
S1 O4 . 1.4510(15) ?
S1 O5 . 1.4585(15) ?
S1 C15 . 1.7808(18) ?
S1 Na2 2_756 3.2984(9) ?
Na2 O5 4_565 2.2500(16) ?
Na2 O4 2_746 2.2602(16) ?
Na2 O3 . 2.4248(15) ?
Na2 N7 . 2.4690(18) ?
Na2 N11 . 2.487(2) ?
Na2 Na2 3_756 3.9829(15) ?
O3 C12 . 1.354(2) ?
O3 H3 . 0.88(3) ?
N7 C19 . 1.312(3) ?
N7 C20 . 1.373(2) ?
N8 C22 . 1.449(2) ?
N8 C28 . 1.461(2) ?
N8 C21 . 1.466(2) ?
N9 C23 . 1.337(3) ?
N9 C27 . 1.350(3) ?
N10 C29 . 1.338(3) ?
N10 C33 . 1.347(3) ?
N11 C34 . 1.129(3) ?
C12 C13 . 1.386(3) ?
C12 C20 . 1.433(3) ?
C13 C14 . 1.411(3) ?
C13 C21 . 1.504(3) ?
C14 C15 . 1.367(3) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.427(3) ?
C16 C20 . 1.413(3) ?
C16 C17 . 1.423(3) ?
C17 C18 . 1.356(3) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.405(3) ?
C18 H18 . 0.9500 ?
C19 H19 . 0.9500 ?
C21 H21A . 0.9900 ?
C21 H21B . 0.9900 ?
C22 C23 . 1.515(3) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C23 C24 . 1.390(3) ?
C24 C25 . 1.383(3) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.380(3) ?
C25 H25 . 0.9500 ?
C26 C27 . 1.380(3) ?
C26 H26 . 0.9500 ?
C27 H27 . 0.9500 ?
C28 C29 . 1.504(3) ?
C28 H28A . 0.9900 ?
C28 H28B . 0.9900 ?
C29 C30 . 1.388(3) ?
C30 C31 . 1.386(3) ?
C30 H30 . 0.9500 ?
C31 C32 . 1.372(3) ?
C31 H31 . 0.9500 ?
C32 C33 . 1.369(4) ?
C32 H32 . 0.9500 ?
C33 H33 . 0.9500 ?
C34 C35 . 1.459(4) ?
C35 H35A . 0.9800 ?
C35 H35B . 0.9800 ?
C35 H35C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O3 H3 N8 . . . 0.88(2) 2.46(3) 3.057(2) 125(2) yes
O3 H3 N9 . . . 0.88(2) 1.87(2) 2.7120(19) 158(3) yes
C31 H31 O6 . . 2_746 0.95 2.53 3.397(3) 152 yes
C35 H35A O6 . . 2_846 0.98 2.55 3.502(4) 166 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O6 S1 O4 Na2 . . . 2_756 -146.44(9) ?
O5 S1 O4 Na2 . . . 2_756 -16.08(13) ?
C15 S1 O4 Na2 . . . 2_756 97.84(10) ?
O6 S1 O5 Na2 . . . 4_566 78.3(2) ?
O4 S1 O5 Na2 . . . 4_566 -52.0(2) ?
C15 S1 O5 Na2 . . . 4_566 -166.41(18) ?
Na2 S1 O5 Na2 2_756 . . 4_566 -61.26(19) ?
Na2 O3 C12 C13 . . . . -167.32(14) ?
Na2 O3 C12 C20 . . . . 14.4(2) ?
O3 C12 C13 C14 . . . . -179.49(17) ?
C20 C12 C13 C14 . . . . -1.2(3) ?
O3 C12 C13 C21 . . . . 1.3(3) ?
C20 C12 C13 C21 . . . . 179.60(16) ?
C12 C13 C14 C15 . . . . 1.6(3) ?
C21 C13 C14 C15 . . . . -179.20(17) ?
C13 C14 C15 C16 . . . . -0.9(3) ?
C13 C14 C15 S1 . . . . 179.41(14) ?
O6 S1 C15 C14 . . . . -126.08(15) ?
O4 S1 C15 C14 . . . . -5.59(17) ?
O5 S1 C15 C14 . . . . 113.80(16) ?
Na2 S1 C15 C14 2_756 . . . 30.51(16) ?
O6 S1 C15 C16 . . . . 54.26(17) ?
O4 S1 C15 C16 . . . . 174.74(15) ?
O5 S1 C15 C16 . . . . -65.86(17) ?
Na2 S1 C15 C16 2_756 . . . -149.16(13) ?
C14 C15 C16 C20 . . . . -0.1(3) ?
S1 C15 C16 C20 . . . . 179.53(13) ?
C14 C15 C16 C17 . . . . 179.75(18) ?
S1 C15 C16 C17 . . . . -0.6(3) ?
C20 C16 C17 C18 . . . . 1.6(3) ?
C15 C16 C17 C18 . . . . -178.31(19) ?
C16 C17 C18 C19 . . . . -0.9(3) ?
C20 N7 C19 C18 . . . . 1.9(3) ?
Na2 N7 C19 C18 . . . . -166.24(17) ?
C17 C18 C19 N7 . . . . -0.9(4) ?
C19 N7 C20 C16 . . . . -1.1(3) ?
Na2 N7 C20 C16 . . . . 167.84(13) ?
C19 N7 C20 C12 . . . . 177.74(18) ?
Na2 N7 C20 C12 . . . . -13.3(2) ?
C17 C16 C20 N7 . . . . -0.6(3) ?
C15 C16 C20 N7 . . . . 179.29(17) ?
C17 C16 C20 C12 . . . . -179.41(17) ?
C15 C16 C20 C12 . . . . 0.5(3) ?
O3 C12 C20 N7 . . . . -0.3(2) ?
C13 C12 C20 N7 . . . . -178.66(16) ?
O3 C12 C20 C16 . . . . 178.61(16) ?
C13 C12 C20 C16 . . . . 0.2(3) ?
C22 N8 C21 C13 . . . . -163.21(16) ?
C28 N8 C21 C13 . . . . 70.82(19) ?
C12 C13 C21 N8 . . . . 63.1(2) ?
C14 C13 C21 N8 . . . . -116.12(18) ?
C28 N8 C22 C23 . . . . -155.23(16) ?
C21 N8 C22 C23 . . . . 78.5(2) ?
C27 N9 C23 C24 . . . . -1.4(3) ?
C27 N9 C23 C22 . . . . 176.90(19) ?
N8 C22 C23 N9 . . . . 6.4(3) ?
N8 C22 C23 C24 . . . . -175.17(18) ?
N9 C23 C24 C25 . . . . 1.3(3) ?
C22 C23 C24 C25 . . . . -177.0(2) ?
C23 C24 C25 C26 . . . . 0.1(3) ?
C24 C25 C26 C27 . . . . -1.3(3) ?
C23 N9 C27 C26 . . . . 0.2(3) ?
C25 C26 C27 N9 . . . . 1.2(4) ?
C22 N8 C28 C29 . . . . 72.0(2) ?
C21 N8 C28 C29 . . . . -161.71(16) ?
C33 N10 C29 C30 . . . . 0.6(3) ?
C33 N10 C29 C28 . . . . -178.2(2) ?
N8 C28 C29 N10 . . . . -145.01(18) ?
N8 C28 C29 C30 . . . . 36.2(3) ?
N10 C29 C30 C31 . . . . -0.4(3) ?
C28 C29 C30 C31 . . . . 178.36(19) ?
C29 C30 C31 C32 . . . . -0.3(3) ?
C30 C31 C32 C33 . . . . 0.7(3) ?
C29 N10 C33 C32 . . . . -0.2(4) ?
C31 C32 C33 N10 . . . . -0.4(4) ?
_cod_database_fobs_code 2022822