#------------------------------------------------------------------------------
#$Date: 2020-08-07 06:26:32 +0300 (Fri, 07 Aug 2020) $
#$Revision: 255165 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/88/1558816.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_1558816
loop_
_publ_author_name
'Ibragimov, Avazbek'
_publ_section_title
;
Bis(3,5-dinitrobenzoato-\kO)bis(ethane-1,2-diamine-\k^2^N,N')cadmium(II)
;
_journal_coeditor_code WM4132
_journal_issue 7
_journal_name_full IUCrData
_journal_page_first x200843
_journal_paper_doi 10.1107/S2414314620008433
_journal_volume 5
_journal_year 2020
_chemical_formula_iupac '[Cd (C7 H3 N2 O6)2 (C2 H8 N2)2)]'
_chemical_formula_moiety 'C18 H22 Cd N8 O12'
_chemical_formula_sum 'C18 H22 Cd N8 O12'
_chemical_formula_weight 654.83
_chemical_name_systematic
Bis(3,5-dinitrobenzoato-\kO)bis(ethane-1,2-diamine-\k^2^N,N')cadmium(II)
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary Intrinsic-phasing
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 112.289(5)
_cell_angle_beta 92.827(5)
_cell_angle_gamma 101.656(5)
_cell_formula_units_Z 1
_cell_length_a 7.191(5)
_cell_length_b 8.698(5)
_cell_length_c 10.987(5)
_cell_measurement_reflns_used 3166
_cell_measurement_temperature 291(2)
_cell_measurement_theta_max 75.1240
_cell_measurement_theta_min 4.3670
_cell_volume 616.7(6)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 291(2)
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type 'Rigaku Oxford Diffraction Xcalibur, Ruby'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0305
_diffrn_reflns_av_unetI/netI 0.0320
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 4512
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.828
_diffrn_reflns_theta_min 4.392
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 7.810
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.39655
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.763
_exptl_crystal_description block
_exptl_crystal_F_000 330
_exptl_crystal_size_max 0.220
_exptl_crystal_size_mid 0.180
_exptl_crystal_size_min 0.160
_refine_diff_density_max 0.448
_refine_diff_density_min -0.506
_refine_ls_extinction_coef 0.0032(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 195
_refine_ls_number_reflns 2482
_refine_ls_number_restraints 5
_refine_ls_restrained_S_all 1.059
_refine_ls_R_factor_all 0.0342
_refine_ls_R_factor_gt 0.0327
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.2183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0846
_refine_ls_wR_factor_ref 0.0864
_reflns_number_gt 2406
_reflns_number_total 2482
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm4132sup1.cif
_cod_data_source_block I
_cod_database_code 1558816
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.278
_shelx_estimated_absorpt_t_max 0.368
_shelx_hkl_file
;
0 0 -1 94.56 1.14
0 0 -1 102.97 1.66
0 0 -1 97.27 1.37
0 0 1 95.98 1.25
0 0 1 91.27 1.19
0 0 1 94.31 1.22
0 0 1 95.99 1.61
0 0 -1 102.02 1.24
0 0 -2 169.90 2.13
0 0 -2 171.98 2.60
0 0 2 169.53 2.42
0 0 2 173.72 2.37
0 0 -2 179.24 1.93
0 0 -3 612.74 6.18
0 0 3 605.24 5.49
0 0 -4 619.57 7.49
0 0 4 619.13 6.56
0 0 -5 1803.94 15.30
0 0 5 1784.07 12.87
0 0 -6 292.04 7.18
0 0 -7 87.64 4.70
0 0 8 147.55 6.11
0 0 8 140.98 5.83
0 0 9 149.32 6.63
0 0 9 142.11 6.33
0 0 10 116.49 5.81
0 0 10 113.12 6.12
0 0 10 110.06 5.79
0 0 11 44.34 3.78
0 0 11 34.93 2.84
0 0 11 37.88 3.44
0 0 12 40.88 2.65
0 0 12 35.24 2.45
0 -1 12 20.82 2.53
0 -1 12 18.48 2.51
0 -1 12 18.40 2.31
0 -1 11 133.63 5.77
0 -1 11 134.75 5.86
0 -1 10 36.71 3.85
0 -1 10 42.75 4.17
0 -1 10 36.73 3.81
0 -1 10 31.93 3.71
0 -1 9 154.64 6.69
0 -1 9 161.01 6.96
0 -1 9 161.87 6.65
0 -1 8 65.47 3.95
0 -1 8 67.76 4.18
0 1 -7 531.45 9.98
0 1 -6 33.22 2.38
0 -1 6 34.99 2.17
0 1 -5 801.36 9.12
0 -1 5 815.09 8.51
0 1 -4 386.30 5.48
0 -1 4 395.93 5.09
0 -1 4 392.07 5.90
0 -1 3 413.38 5.01
0 -1 3 420.38 4.38
0 -1 2 903.34 5.02
0 1 -2 895.33 5.67
0 -1 1 1511.55 16.82
0 -1 1 1486.29 6.08
0 -1 1 1504.82 6.54
0 -1 0 573.52 3.04
0 1 0 566.59 3.41
0 1 0 577.03 3.10
0 1 1 2498.44 10.34
0 -1 -1 2400.60 11.27
0 1 1 2489.38 29.58
0 1 1 2410.83 26.71
0 -1 -1 2575.12 7.36
0 1 2 553.86 4.66
0 1 2 543.48 5.00
0 1 2 556.86 4.42
0 -1 -3 97.90 3.44
0 1 3 91.41 2.29
0 1 3 95.17 2.63
0 -1 -4 1247.52 13.42
0 1 4 1228.00 10.58
0 1 4 1207.33 9.52
0 -1 -5 531.95 9.92
0 1 5 516.30 7.22
0 -1 -6 166.91 6.31
0 1 7 169.38 6.01
0 1 7 162.36 6.88
0 1 7 162.28 5.64
0 1 8 175.87 6.70
0 1 9 128.91 6.45
0 1 9 134.10 6.24
0 1 10 78.85 4.80
0 1 10 90.99 5.33
0 1 11 19.66 2.59
0 1 11 20.61 2.58
0 -2 13 33.00 2.21
0 -2 12 9.83 2.36
0 -2 12 12.60 2.58
0 -2 11 40.70 3.98
0 -2 11 38.04 3.74
0 -2 10 128.52 6.27
0 -2 10 128.74 6.52
0 -2 10 118.69 6.23
0 -2 9 242.93 8.12
0 -2 9 229.56 8.25
0 -2 9 235.65 7.73
0 2 -8 198.37 6.65
0 2 -7 17.35 2.03
0 -2 6 605.01 9.11
0 2 -6 601.25 8.80
0 -2 5 472.81 6.27
0 -2 5 463.54 7.06
0 -2 4 641.39 7.07
0 -2 4 647.33 6.26
0 -2 3 343.82 3.77
0 -2 3 322.19 4.46
0 -2 2 287.97 4.27
0 -2 2 271.85 3.77
0 2 -1 1596.20 7.30
0 -2 1 1610.50 7.09
0 -2 0 168.71 2.45
0 2 0 161.82 1.77
0 2 0 169.75 2.73
0 2 1 815.70 4.08
0 2 1 802.49 5.01
0 -2 -1 803.11 6.00
0 -2 -1 801.00 6.17
0 2 2 34.87 1.73
0 -2 -2 39.54 2.02
0 -2 -2 36.60 1.65
0 2 2 32.44 1.37
0 2 2 42.24 1.27
0 2 2 35.64 1.26
0 2 3 538.49 6.98
0 2 3 561.50 5.70
0 -2 -4 108.93 4.39
0 2 4 109.57 3.69
0 -2 -5 7.44 2.38
0 -2 -5 2.98 1.29
0 -2 -6 127.09 4.61
0 2 7 252.09 7.23
0 2 7 250.92 7.68
0 2 7 241.56 8.65
0 2 8 81.62 4.66
0 2 9 30.27 3.43
0 2 9 27.62 3.71
0 2 9 28.37 3.22
0 2 10 25.47 2.95
0 2 10 11.03 2.84
0 2 11 33.66 2.63
0 -3 13 14.61 1.81
0 -3 12 113.31 5.40
0 -3 12 106.40 5.31
0 -3 11 62.55 4.48
0 -3 11 53.77 4.93
0 -3 10 70.29 5.31
0 -3 10 70.72 4.61
0 -3 9 126.53 6.45
0 -3 9 114.12 5.94
0 -3 9 119.25 5.57
0 3 -8 476.21 9.74
0 3 -7 166.66 5.29
0 -3 7 163.54 5.26
0 -3 6 658.95 9.27
0 3 -6 727.94 9.94
0 -3 5 157.54 4.09
0 -3 4 1062.72 9.54
0 -3 3 642.56 7.06
0 -3 3 631.77 7.28
0 -3 2 364.96 5.36
0 -3 2 365.18 5.04
0 -3 1 2089.99 10.13
0 3 -1 2064.42 10.93
0 -3 0 1013.96 7.46
0 3 0 1035.57 5.32
0 -3 -1 809.11 7.40
0 3 1 857.13 5.85
0 3 2 515.34 7.06
0 3 2 520.23 5.49
0 -3 -2 513.45 6.69
0 3 3 265.37 5.75
0 -3 -3 253.82 5.23
0 3 4 137.44 4.59
0 -3 -4 129.15 4.11
0 3 5 190.94 6.88
0 3 5 189.02 5.80
0 3 6 190.77 6.53
0 3 6 187.97 7.35
0 3 6 199.87 6.01
0 3 7 23.48 3.10
0 3 7 24.86 3.34
0 3 7 23.62 2.92
0 3 8 61.91 3.78
0 3 9 23.94 3.15
0 3 9 22.21 3.13
0 3 10 29.33 2.77
0 -4 13 68.86 3.59
0 -4 12 55.69 4.07
0 -4 11 31.52 3.47
0 -4 10 71.33 4.56
0 -4 10 76.66 5.49
0 -4 9 226.21 7.27
0 -4 9 213.88 7.71
0 -4 8 368.38 9.32
0 -4 8 372.50 8.54
0 -4 8 368.65 8.52
0 4 -7 450.35 8.81
0 -4 7 396.97 8.12
0 -4 6 184.10 5.04
0 4 -5 195.41 3.78
0 -4 5 206.89 4.96
0 -4 4 74.55 3.00
0 -4 4 79.77 2.75
0 -4 3 673.22 8.22
0 4 -3 647.97 6.73
0 -4 2 1393.10 10.91
0 -4 2 1372.16 12.27
0 4 -1 354.11 2.97
0 -4 1 342.05 5.02
0 -4 0 66.61 2.41
0 -4 -1 939.85 9.52
0 4 1 928.00 10.09
0 4 2 627.25 8.95
0 -4 -2 638.06 8.52
0 4 3 440.92 8.29
0 -4 -3 407.37 7.39
0 4 4 78.05 4.61
0 4 4 87.96 3.94
0 4 5 127.70 6.19
0 4 5 126.33 5.14
0 4 6 141.86 6.77
0 4 6 130.52 5.65
0 4 7 118.05 6.21
0 4 8 48.13 3.75
0 4 9 11.17 2.15
0 4 9 3.45 2.74
0 -5 13 54.53 3.14
0 -5 12 32.41 3.14
0 -5 11 11.01 2.54
0 -5 10 106.90 5.43
0 -5 10 97.85 5.03
0 -5 9 137.81 5.66
0 -5 8 312.10 7.64
0 5 -7 162.65 5.63
0 -5 7 160.45 5.49
0 -5 6 81.02 3.67
0 5 -5 374.42 5.79
0 -5 5 393.04 7.33
0 -5 4 224.07 5.57
0 5 -4 185.35 4.19
0 5 -3 117.67 3.38
0 -5 3 124.85 4.12
0 -5 2 72.41 3.42
0 -5 1 29.44 1.90
0 -5 0 521.74 7.77
0 5 0 489.72 7.87
0 5 1 202.31 5.36
0 -5 -1 212.08 5.25
0 5 2 122.02 5.44
0 -5 -2 115.78 4.07
0 5 3 140.89 6.15
0 5 3 146.99 4.91
0 5 4 2.55 2.43
0 5 4 2.60 2.80
0 5 5 71.60 5.23
0 5 5 68.86 3.97
0 5 6 143.72 6.80
0 5 7 48.48 4.01
0 5 7 49.11 3.39
0 5 8 6.02 2.17
0 5 8 2.29 2.30
0 -6 13 38.21 2.14
0 -6 13 34.10 2.05
0 -6 12 32.29 2.80
0 -6 11 29.11 2.91
0 -6 11 37.97 3.27
0 -6 10 45.39 3.71
0 -6 10 50.38 3.73
0 -6 9 78.85 4.26
0 -6 9 71.40 4.32
0 -6 8 119.37 5.28
0 -6 7 156.43 5.61
0 -6 6 233.15 6.53
0 -6 5 142.01 4.83
0 -6 4 233.58 6.21
0 -6 3 66.60 3.42
0 -6 2 136.15 5.09
0 6 -1 137.53 4.55
0 6 0 133.39 5.78
0 6 0 148.80 4.87
0 6 1 178.03 5.88
0 6 1 143.87 6.44
0 6 2 260.87 8.69
0 6 2 253.75 7.14
0 6 3 70.37 4.84
0 6 3 68.50 3.65
0 6 4 98.83 5.57
0 6 4 108.97 4.69
0 6 5 48.60 4.03
0 6 6 12.36 2.43
0 6 6 11.61 2.64
0 6 7 15.63 1.93
0 -7 13 43.31 2.07
0 -7 12 11.39 2.28
0 -7 11 58.49 3.79
0 -7 10 73.02 4.57
0 -7 9 129.49 5.73
0 -7 9 117.78 5.66
0 -7 8 33.32 3.32
0 -7 8 25.23 2.91
0 -7 7 139.29 5.67
0 -7 6 122.33 5.15
0 -7 5 176.70 5.91
0 -7 5 169.29 5.82
0 -7 4 27.35 2.95
0 7 -4 28.06 2.97
0 -7 4 27.06 2.84
0 -7 3 259.78 6.70
0 7 -3 277.52 8.39
0 -7 2 54.57 3.21
0 7 -2 57.04 4.12
0 7 -1 52.44 4.09
0 7 -1 57.90 3.33
0 7 0 207.57 7.85
0 7 0 236.97 6.74
0 7 1 43.63 3.32
0 7 1 37.15 3.81
0 7 2 121.16 6.26
0 7 3 70.88 4.81
0 7 4 12.15 2.62
0 7 5 22.32 2.62
0 -8 12 24.57 1.79
0 -8 11 62.23 3.68
0 -8 10 23.66 2.79
0 -8 9 84.23 4.90
0 -8 8 46.79 3.71
0 -8 7 78.06 4.46
0 -8 7 71.02 4.27
0 8 -6 76.56 4.89
0 -8 6 80.58 4.47
0 -8 6 78.93 4.40
0 8 -5 108.74 5.85
0 -8 5 113.45 4.95
0 -8 5 104.28 4.66
0 -8 4 87.31 4.39
0 8 -4 102.95 5.80
0 8 -3 23.56 3.28
0 8 -2 65.12 4.73
0 8 -2 53.99 4.48
0 8 -1 52.35 4.42
0 8 0 13.31 2.80
0 8 1 174.51 7.05
0 8 2 2.57 2.21
0 8 3 29.51 2.99
0 8 4 18.32 1.94
0 -9 11 7.62 1.68
0 9 -11 7.11 1.71
0 -9 11 9.70 1.66
0 9 -10 41.03 3.04
0 -9 10 49.46 3.18
0 9 -9 0.25 2.24
0 -9 9 1.57 1.90
0 9 -8 32.66 3.25
0 -9 8 35.07 3.20
0 -9 7 52.67 3.46
0 9 -7 53.13 4.03
0 9 -6 78.99 4.89
0 -9 6 78.01 4.09
0 9 -5 2.53 2.49
0 9 -4 63.95 4.39
0 9 -4 52.81 4.22
0 9 -3 33.22 4.28
0 9 -3 39.24 3.87
0 9 -2 34.68 3.72
0 9 -1 24.44 2.99
0 9 0 9.82 2.09
0 9 1 18.33 2.33
0 9 2 7.29 1.69
0 -10 9 11.55 1.72
0 10 -9 10.28 1.86
0 10 -9 12.32 1.75
0 10 -8 25.19 2.39
0 -10 8 23.32 1.99
0 10 -8 25.73 2.43
0 10 -7 27.07 2.51
0 -10 7 25.68 2.38
0 10 -7 25.06 2.48
0 10 -6 10.97 2.08
0 10 -6 8.92 2.70
0 10 -5 20.57 3.27
0 10 -5 17.91 2.47
0 10 -4 11.13 2.21
0 10 -3 20.74 2.37
0 10 -2 24.01 2.26
0 10 -1 6.89 1.76
-1 10 -1 18.85 1.81
-1 10 -2 27.45 2.29
-1 10 -3 14.25 2.17
-1 10 -3 18.09 3.61
-1 10 -4 12.59 3.15
-1 10 -4 18.67 2.30
-1 10 -5 22.27 2.83
-1 10 -5 24.98 2.54
1 -10 6 37.85 2.57
-1 10 -6 39.78 3.37
-1 10 -6 38.31 2.76
-1 10 -7 14.45 2.11
-1 10 -7 11.59 2.42
1 -10 7 13.07 2.15
1 -10 8 13.80 1.88
-1 10 -8 10.84 2.38
-1 10 -8 11.54 2.02
-1 10 -9 34.08 2.49
1 -10 9 33.96 2.38
-1 9 2 10.92 1.79
-1 9 1 8.72 1.93
-1 9 0 6.04 2.26
-1 9 -1 42.20 3.57
-1 9 -1 59.49 4.46
-1 9 -2 36.68 3.72
-1 9 -2 29.96 3.19
-1 9 -3 24.27 3.34
-1 9 -3 23.06 3.01
-1 9 -4 19.72 3.10
-1 9 -4 17.60 2.60
1 -9 5 37.33 2.89
-1 9 -5 40.08 3.32
1 -9 6 61.65 3.64
-1 9 -6 63.83 3.98
1 -9 7 41.71 3.17
-1 9 -7 41.60 3.53
1 -9 8 16.95 2.46
-1 9 -8 21.67 2.60
-1 9 -9 45.92 3.17
1 -9 9 48.01 2.69
1 -9 9 42.35 3.12
1 -9 10 40.27 2.69
1 -9 10 34.19 2.81
-1 9 -10 32.58 2.38
1 -9 11 21.42 1.82
1 -9 11 22.85 2.14
-1 8 4 42.66 2.75
-1 8 3 20.73 2.58
-1 8 2 39.85 3.44
-1 8 1 35.46 3.49
-1 8 0 69.61 4.47
-1 8 0 102.03 5.61
-1 8 -1 153.43 6.51
-1 8 -1 126.75 5.94
-1 8 -2 63.16 4.13
-1 8 -2 55.07 4.05
-1 8 -3 45.86 3.60
1 -8 4 34.53 3.02
-1 8 -4 29.86 3.09
1 -8 5 66.30 3.70
-1 8 -5 77.43 4.54
1 -8 6 88.49 4.53
-1 8 -6 89.22 4.95
1 -8 7 45.97 3.53
1 -8 8 59.55 3.97
1 -8 9 36.61 3.17
1 -8 10 80.35 4.52
1 -8 11 35.43 2.96
1 -8 12 10.13 1.78
-1 7 6 27.79 2.08
-1 7 5 29.42 2.81
-1 7 4 17.75 2.69
-1 7 3 59.98 4.29
-1 7 2 60.47 4.34
-1 7 1 80.12 5.12
-1 7 1 58.91 4.43
-1 7 0 194.26 7.11
-1 7 0 202.66 7.43
-1 7 -1 189.34 6.91
-1 7 -1 197.91 6.88
-1 7 -2 310.51 8.40
1 -7 3 27.27 3.07
-1 7 -3 26.80 2.98
1 -7 4 176.04 5.55
-1 7 -4 182.92 6.32
1 -7 4 193.12 5.78
1 -7 5 184.22 5.88
1 -7 5 195.68 6.04
1 -7 6 183.01 6.11
1 -7 6 177.34 6.00
1 -7 7 5.64 2.19
1 -7 8 202.73 6.97
1 -7 9 81.53 4.67
1 -7 10 35.88 3.22
1 -7 11 60.17 3.71
1 -7 12 21.28 2.27
-1 6 7 31.19 2.65
-1 6 6 21.78 2.88
-1 6 6 18.72 2.89
-1 6 5 31.99 3.46
-1 6 5 31.60 3.15
-1 6 4 1.11 2.57
-1 6 3 222.53 7.94
-1 6 2 29.24 3.33
-1 6 1 80.36 5.22
-1 6 1 68.22 4.29
-1 6 0 100.24 4.79
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_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 79460
_shelx_res_file
;
TITL I
1266.res
created by SHELXL-2018/3 at 23:18:33 on 16-Apr-2020
CELL 1.54184 7.191 8.698 10.987 112.289 92.827 101.656
ZERR 1 0.005 0.005 0.005 0.005 0.005 0.005
LATT 1
SFAC C H Cd N O
UNIT 18 22 1 8 12
DFIX 0.92 0.01 N3 H3a N3 H3b N4 H4b N4 H4a
DFIX 1.5 H3a H3b
L.S. 4
PLAN 5
SIZE 0.22 0.18 0.16
TEMP 18
CONF
HTAB N4 O2
EQIV $2 -x+1, -y+1, -z+1
HTAB N4 O4_$2
EQIV $3 x+1, y+1, z+1
HTAB N4 O4_$3
EQIV $4 -x+2, -y, -z+1
HTAB N3 O5_$4
HTAB
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
WGHT 0.051300 0.218300
EXTI 0.003155
FVAR 0.67368
CD1 3 1.000000 0.500000 1.000000 10.50000 0.05393 0.04609 =
0.03613 0.01752 0.00951 0.01547
O2 5 0.654925 0.543292 0.793005 11.00000 0.05237 0.06988 =
0.05086 -0.00347 -0.00219 0.02367
O1 5 0.821568 0.349274 0.788107 11.00000 0.07443 0.06498 =
0.04184 0.01443 -0.00960 0.02437
O3 5 0.123257 0.337321 0.429070 11.00000 0.05560 0.08642 =
0.07436 0.02786 -0.00125 0.03183
O4 5 0.128195 0.127789 0.244952 11.00000 0.07563 0.06645 =
0.07115 0.01806 -0.03542 0.01036
O6 5 0.856533 -0.092702 0.359432 11.00000 0.06845 0.07796 =
0.07440 0.02087 0.01027 0.04034
N1 4 0.197849 0.228352 0.358305 11.00000 0.04640 0.05346 =
0.05540 0.02567 -0.00754 0.00802
N4 4 1.022154 0.765105 0.990364 11.00000 0.05581 0.04368 =
0.04280 0.00993 0.00137 0.01923
O5 5 0.664315 -0.137021 0.188215 11.00000 0.09567 0.07106 =
0.04812 0.00401 0.01402 0.03160
N2 4 0.725814 -0.060886 0.305728 11.00000 0.05613 0.04716 =
0.04945 0.01542 0.01623 0.01359
C2 1 0.627126 0.299964 0.593961 11.00000 0.03651 0.04197 =
0.03560 0.01686 0.00381 0.00618
C3 1 0.460253 0.320772 0.539802 11.00000 0.03842 0.04082 =
0.04002 0.01716 0.00555 0.00845
AFIX 43
H3 2 0.402141 0.406126 0.589595 11.00000 -1.20000
AFIX 0
C7 1 0.715494 0.174275 0.516446 11.00000 0.03851 0.04367 =
0.03878 0.01855 0.00523 0.01094
AFIX 43
H7 2 0.827318 0.158989 0.551588 11.00000 -1.20000
AFIX 0
C6 1 0.634013 0.073290 0.386932 11.00000 0.04460 0.03741 =
0.03807 0.01610 0.00861 0.00902
C4 1 0.382246 0.213216 0.411400 11.00000 0.03936 0.04117 =
0.04146 0.02077 -0.00176 0.00628
C5 1 0.466170 0.088300 0.331967 11.00000 0.04830 0.04002 =
0.03498 0.01387 0.00110 0.00428
AFIX 43
H5 2 0.411582 0.017367 0.245051 11.00000 -1.20000
AFIX 0
N3 4 1.244863 0.515209 0.869766 11.00000 0.06752 0.07266 =
0.09753 0.04678 0.03813 0.03548
C1 1 0.708441 0.410053 0.738993 11.00000 0.03859 0.05229 =
0.03498 0.01115 0.00340 0.00831
C8 1 1.203253 0.809662 0.942711 11.00000 0.06396 0.05249 =
0.07444 0.03294 0.00484 0.00882
AFIX 23
H8A 2 1.307671 0.851575 1.015179 11.00000 -1.20000
H8B 2 1.200122 0.900523 0.912486 11.00000 -1.20000
AFIX 0
C9 1 1.238022 0.659406 0.832114 11.00000 0.07381 0.08564 =
0.08236 0.05183 0.03454 0.02891
AFIX 23
H9A 2 1.136935 0.622053 0.758114 11.00000 -1.20000
H9B 2 1.358522 0.693491 0.802584 11.00000 -1.20000
AFIX 0
H4A 2 0.922448 0.747150 0.927572 11.00000 0.05013
H4B 2 1.023570 0.846063 1.073634 11.00000 0.07202
H3A 2 1.336493 0.585800 0.940240 11.00000 0.05252
H3B 2 1.285476 0.419423 0.821346 11.00000 0.26689
HKLF 4
REM I
REM wR2 = 0.0864, GooF = S = 1.060, Restrained GooF = 1.059 for all data
REM R1 = 0.0327 for 2406 Fo > 4sig(Fo) and 0.0342 for all 2482 data
REM 195 parameters refined using 5 restraints
END
WGHT 0.0513 0.2183
REM Instructions for potential hydrogen bonds
HTAB N4 O2
HTAB N4 O4_$2
HTAB N4 O4_$3
HTAB N3 O5_$4
REM Highest difference peak 0.448, deepest hole -0.506, 1-sigma level 0.072
Q1 1 1.3330 0.7105 0.9274 11.00000 0.05 0.45
Q2 1 1.1125 0.4246 0.9393 11.00000 0.05 0.39
Q3 1 1.3645 0.4938 0.8897 11.00000 0.05 0.34
Q4 1 1.1763 0.3844 0.7757 11.00000 0.05 0.32
Q5 1 0.8864 0.3539 0.8671 11.00000 0.05 0.30
;
_shelx_res_checksum 3313
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Cd Cd1 1.000000 0.500000 1.000000 0.04436(14) Uani d 1 . .
O O2 0.6549(4) 0.5433(4) 0.7930(3) 0.0651(7) Uani d 1 . .
O O1 0.8216(4) 0.3493(3) 0.7881(2) 0.0620(7) Uani d 1 . .
O O3 0.1233(4) 0.3373(4) 0.4291(3) 0.0715(8) Uani d 1 . .
O O4 0.1282(4) 0.1278(4) 0.2450(3) 0.0767(9) Uani d 1 . .
O O6 0.8565(4) -0.0927(4) 0.3594(3) 0.0730(8) Uani d 1 . .
N N1 0.1978(4) 0.2284(4) 0.3583(3) 0.0517(6) Uani d 1 . .
N N4 1.0222(4) 0.7651(3) 0.9904(3) 0.0487(6) Uani d 1 . .
O O5 0.6643(5) -0.1370(4) 0.1882(3) 0.0757(8) Uani d 1 . .
N N2 0.7258(4) -0.0609(4) 0.3057(3) 0.0516(6) Uani d 1 . .
C C2 0.6271(4) 0.3000(4) 0.5940(3) 0.0381(6) Uani d 1 . .
C C3 0.4603(4) 0.3208(4) 0.5398(3) 0.0396(6) Uani d 1 . .
H H3 0.402141 0.406126 0.589595 0.047 Uiso calc 1 . .
C C7 0.7155(4) 0.1743(4) 0.5164(3) 0.0395(6) Uani d 1 . .
H H7 0.827318 0.158989 0.551588 0.047 Uiso calc 1 . .
C C6 0.6340(4) 0.0733(4) 0.3869(3) 0.0397(6) Uani d 1 . .
C C4 0.3822(4) 0.2132(4) 0.4114(3) 0.0401(6) Uani d 1 . .
C C5 0.4662(4) 0.0883(4) 0.3320(3) 0.0426(6) Uani d 1 . .
H H5 0.411582 0.017367 0.245051 0.051 Uiso calc 1 . .
N N3 1.2449(5) 0.5152(5) 0.8698(4) 0.0714(10) Uani d 1 . .
C C1 0.7084(4) 0.4101(4) 0.7390(3) 0.0443(7) Uani d 1 . .
C C8 1.2033(6) 0.8097(5) 0.9427(4) 0.0622(9) Uani d 1 . .
H H8A 1.307671 0.851575 1.015179 0.075 Uiso calc 1 . .
H H8B 1.200122 0.900523 0.912486 0.075 Uiso calc 1 . .
C C9 1.2380(7) 0.6594(6) 0.8321(5) 0.0725(11) Uani d 1 . .
H H9A 1.136935 0.622053 0.758114 0.087 Uiso calc 1 . .
H H9B 1.358522 0.693491 0.802584 0.087 Uiso calc 1 . .
H H4A 0.922(4) 0.747(5) 0.928(3) 0.050(10) Uiso d 1 . .
H H4B 1.024(6) 0.846(4) 1.074(2) 0.072(13) Uiso d 1 . .
H H3A 1.336(4) 0.586(4) 0.940(3) 0.053(11) Uiso d 1 . .
H H3B 1.285(10) 0.419(8) 0.821(8) 0.27(6) 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
Cd1 0.0539(2) 0.0461(2) 0.03613(18) 0.01547(13) 0.00951(12) 0.01752(13)
O2 0.0524(14) 0.0699(16) 0.0509(13) 0.0237(12) -0.0022(10) -0.0035(12)
O1 0.0744(17) 0.0650(15) 0.0418(12) 0.0244(13) -0.0096(11) 0.0144(11)
O3 0.0556(15) 0.086(2) 0.0744(18) 0.0318(14) -0.0012(13) 0.0279(16)
O4 0.0756(19) 0.0665(17) 0.0712(18) 0.0104(14) -0.0354(15) 0.0181(15)
O6 0.0684(17) 0.0780(19) 0.0744(18) 0.0403(15) 0.0103(14) 0.0209(15)
N1 0.0464(14) 0.0535(16) 0.0554(16) 0.0080(12) -0.0075(12) 0.0257(13)
N4 0.0558(16) 0.0437(14) 0.0428(14) 0.0192(12) 0.0014(11) 0.0099(11)
O5 0.096(2) 0.0711(18) 0.0481(15) 0.0316(16) 0.0140(13) 0.0040(13)
N2 0.0561(16) 0.0472(15) 0.0494(15) 0.0136(12) 0.0162(12) 0.0154(12)
C2 0.0365(13) 0.0420(15) 0.0356(13) 0.0062(11) 0.0038(10) 0.0169(12)
C3 0.0384(14) 0.0408(15) 0.0400(14) 0.0085(11) 0.0056(11) 0.0172(12)
C7 0.0385(14) 0.0437(15) 0.0388(14) 0.0109(11) 0.0052(11) 0.0185(12)
C6 0.0446(15) 0.0374(14) 0.0381(14) 0.0090(11) 0.0086(11) 0.0161(12)
C4 0.0394(14) 0.0412(15) 0.0415(14) 0.0063(11) -0.0018(11) 0.0208(12)
C5 0.0483(16) 0.0400(15) 0.0350(13) 0.0043(12) 0.0011(11) 0.0139(12)
N3 0.068(2) 0.073(2) 0.098(3) 0.0355(19) 0.038(2) 0.047(2)
C1 0.0386(14) 0.0523(17) 0.0350(14) 0.0083(12) 0.0034(11) 0.0112(13)
C8 0.064(2) 0.052(2) 0.074(2) 0.0088(16) 0.0048(18) 0.0329(19)
C9 0.074(3) 0.086(3) 0.082(3) 0.029(2) 0.035(2) 0.052(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 Cd1 N4 2_767 . 179.999(11) ?
N4 Cd1 N3 2_767 . 102.66(12) ?
N4 Cd1 N3 . . 77.34(12) ?
N4 Cd1 N3 2_767 2_767 77.34(12) ?
N4 Cd1 N3 . 2_767 102.66(12) ?
N3 Cd1 N3 . 2_767 180.0 ?
N4 Cd1 O1 2_767 . 86.36(10) ?
N4 Cd1 O1 . . 93.64(10) ?
N3 Cd1 O1 . . 80.38(15) ?
N3 Cd1 O1 2_767 . 99.63(15) ?
N4 Cd1 O1 2_767 2_767 93.64(10) ?
N4 Cd1 O1 . 2_767 86.36(10) ?
N3 Cd1 O1 . 2_767 99.62(15) ?
N3 Cd1 O1 2_767 2_767 80.37(15) ?
O1 Cd1 O1 . 2_767 180.00(8) ?
C1 O1 Cd1 . . 122.9(2) ?
O3 N1 O4 . . 124.1(3) ?
O3 N1 C4 . . 118.6(3) ?
O4 N1 C4 . . 117.3(3) ?
C8 N4 Cd1 . . 107.5(2) ?
C8 N4 H4A . . 109(2) ?
Cd1 N4 H4A . . 105(2) ?
C8 N4 H4B . . 109(3) ?
Cd1 N4 H4B . . 110(3) ?
H4A N4 H4B . . 117(4) ?
O5 N2 O6 . . 123.1(3) ?
O5 N2 C6 . . 118.1(3) ?
O6 N2 C6 . . 118.8(3) ?
C3 C2 C7 . . 119.7(3) ?
C3 C2 C1 . . 119.7(3) ?
C7 C2 C1 . . 120.5(3) ?
C4 C3 C2 . . 118.9(3) ?
C4 C3 H3 . . 120.5 ?
C2 C3 H3 . . 120.5 ?
C6 C7 C2 . . 118.8(3) ?
C6 C7 H7 . . 120.6 ?
C2 C7 H7 . . 120.6 ?
C5 C6 C7 . . 122.6(3) ?
C5 C6 N2 . . 118.6(3) ?
C7 C6 N2 . . 118.8(3) ?
C3 C4 C5 . . 122.8(3) ?
C3 C4 N1 . . 118.4(3) ?
C5 C4 N1 . . 118.8(3) ?
C6 C5 C4 . . 117.1(3) ?
C6 C5 H5 . . 121.5 ?
C4 C5 H5 . . 121.5 ?
C9 N3 Cd1 . . 106.2(2) ?
C9 N3 H3A . . 90(3) ?
Cd1 N3 H3A . . 95(3) ?
C9 N3 H3B . . 126(8) ?
Cd1 N3 H3B . . 121(7) ?
H3A N3 H3B . . 110(2) ?
O2 C1 O1 . . 128.6(3) ?
O2 C1 C2 . . 117.4(3) ?
O1 C1 C2 . . 114.0(3) ?
N4 C8 C9 . . 111.1(3) ?
N4 C8 H8A . . 109.4 ?
C9 C8 H8A . . 109.4 ?
N4 C8 H8B . . 109.4 ?
C9 C8 H8B . . 109.4 ?
H8A C8 H8B . . 108.0 ?
N3 C9 C8 . . 112.9(4) ?
N3 C9 H9A . . 109.0 ?
C8 C9 H9A . . 109.0 ?
N3 C9 H9B . . 109.0 ?
C8 C9 H9B . . 109.0 ?
H9A C9 H9B . . 107.8 ?
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
Cd1 N4 2_767 2.322(3) ?
Cd1 N4 . 2.322(3) ?
Cd1 N3 . 2.337(4) ?
Cd1 N3 2_767 2.337(4) ?
Cd1 O1 . 2.344(2) ?
Cd1 O1 2_767 2.344(2) ?
O2 C1 . 1.235(4) ?
O1 C1 . 1.257(4) ?
O3 N1 . 1.216(4) ?
O4 N1 . 1.226(4) ?
O6 N2 . 1.218(4) ?
N1 C4 . 1.473(4) ?
N4 C8 . 1.462(5) ?
N4 H4A . 0.916(10) ?
N4 H4B . 0.917(10) ?
O5 N2 . 1.216(4) ?
N2 C6 . 1.474(4) ?
C2 C3 . 1.388(4) ?
C2 C7 . 1.397(4) ?
C2 C1 . 1.524(4) ?
C3 C4 . 1.374(4) ?
C3 H3 . 0.9300 ?
C7 C6 . 1.379(4) ?
C7 H7 . 0.9300 ?
C6 C5 . 1.375(4) ?
C4 C5 . 1.380(4) ?
C5 H5 . 0.9300 ?
N3 C9 . 1.471(6) ?
N3 H3A . 0.914(10) ?
N3 H3B . 0.916(10) ?
C8 C9 . 1.485(6) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_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
N4 H4A O2 . 0.916(10) 2.32(2) 3.099(4) 143(3) yes
N4 H4A O4 2_666 0.916(10) 2.56(3) 3.268(4) 134(3) yes
N4 H4B O4 1_666 0.917(10) 2.39(2) 3.237(4) 153(4) yes
N3 H3B O5 2_756 0.916(10) 2.52(7) 3.312(5) 145(10) 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
C7 C2 C3 C4 . . . . 1.8(4) ?
C1 C2 C3 C4 . . . . -175.9(3) ?
C3 C2 C7 C6 . . . . 0.0(4) ?
C1 C2 C7 C6 . . . . 177.8(3) ?
C2 C7 C6 C5 . . . . -1.8(4) ?
C2 C7 C6 N2 . . . . -179.2(3) ?
O5 N2 C6 C5 . . . . 9.9(4) ?
O6 N2 C6 C5 . . . . -168.6(3) ?
O5 N2 C6 C7 . . . . -172.6(3) ?
O6 N2 C6 C7 . . . . 8.9(4) ?
C2 C3 C4 C5 . . . . -2.2(4) ?
C2 C3 C4 N1 . . . . 175.6(3) ?
O3 N1 C4 C3 . . . . 1.3(5) ?
O4 N1 C4 C3 . . . . -177.9(3) ?
O3 N1 C4 C5 . . . . 179.2(3) ?
O4 N1 C4 C5 . . . . 0.0(4) ?
C7 C6 C5 C4 . . . . 1.5(4) ?
N2 C6 C5 C4 . . . . 178.9(3) ?
C3 C4 C5 C6 . . . . 0.5(4) ?
N1 C4 C5 C6 . . . . -177.3(3) ?
Cd1 O1 C1 O2 . . . . -8.4(5) ?
Cd1 O1 C1 C2 . . . . 172.57(19) ?
C3 C2 C1 O2 . . . . -19.2(4) ?
C7 C2 C1 O2 . . . . 163.0(3) ?
C3 C2 C1 O1 . . . . 159.9(3) ?
C7 C2 C1 O1 . . . . -17.8(4) ?
Cd1 N4 C8 C9 . . . . 42.2(4) ?
Cd1 N3 C9 C8 . . . . 41.0(5) ?
N4 C8 C9 N3 . . . . -59.1(5) ?
_cod_database_fobs_code 1558816