#------------------------------------------------------------------------------
#$Date: 2021-09-22 04:59:54 +0300 (Wed, 22 Sep 2021) $
#$Revision: 269241 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243923.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_2243923
loop_
_publ_author_name
'Vassilyeva, Olga Yu.'
'Kokozay, Vladimir N.'
'Petrusenko, Svitlana'
'Sobolev, Alexandre N.'
_publ_section_title
;
Crystal structure of
hexakis(N,N-dimethylformamide-\kO)iron(III)
\m-chlorido-bis(trichloridocadmium)
;
_journal_coeditor_code CQ2046
_journal_issue 10
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989021009580
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac '[Fe (C3 H7 N1 O1)6] [Cd2 Cl7]'
_chemical_formula_moiety 'C18 H42 Fe N6 O6 3+, Cd2 Cl7 3-'
_chemical_formula_sum 'C18 H42 Cd2 Cl7 Fe N6 O6'
_chemical_formula_weight 967.37
_chemical_name_systematic
;
Hexakis(N,N-dimethylformamide-\kO)iron(III)
\m-chlorido-bis(trichloridocadmium)
;
_space_group_crystal_system trigonal
_space_group_IT_number 148
_space_group_name_Hall '-R 3'
_space_group_name_H-M_alt 'R -3 :H'
_atom_sites_solution_hydrogens mixed
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 13.7143(2)
_cell_length_b 13.7143
_cell_length_c 16.1312(2)
_cell_measurement_reflns_used 9616
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 67.043
_cell_measurement_theta_min 4.603
_cell_volume 2627.51(5)
_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
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_source 'Enhance (Cu) X-ray Source'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0383
_diffrn_reflns_av_unetI/netI 0.0133
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 16143
_diffrn_reflns_theta_full 67.183
_diffrn_reflns_theta_max 67.183
_diffrn_reflns_theta_min 4.623
_exptl_absorpt_coefficient_mu 18.176
_exptl_absorpt_correction_T_max 1.0
_exptl_absorpt_correction_T_min 0.75984
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour 'dark green'
_exptl_crystal_density_diffrn 1.834
_exptl_crystal_description octahedral
_exptl_crystal_F_000 1443
_exptl_crystal_size_max 0.062
_exptl_crystal_size_mid 0.050
_exptl_crystal_size_min 0.045
_refine_diff_density_max 0.786
_refine_diff_density_min -0.331
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.002
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 67
_refine_ls_number_reflns 1051
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.002
_refine_ls_R_factor_all 0.0221
_refine_ls_R_factor_gt 0.0196
_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/[\s^2^(Fo^2^)+(0.0422P)^2^+4.2200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0555
_refine_ls_wR_factor_ref 0.0574
_reflns_number_gt 980
_reflns_number_total 1051
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file cq2046sup1.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'R -3'
_cod_database_code 2243923
_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 0.399
_shelx_estimated_absorpt_t_max 0.495
_shelx_hkl_file
;
0 0 3 816.91 21.58
0 0 -3 792.14 21.55
0 0 3 883.65 20.90
0 0 3 844.40 21.54
0 0 3 913.99 20.75
0 0 -6 856.15 23.37
0 0 6 885.90 23.27
0 0 -6 906.18 22.84
0 0 -6 873.86 23.46
0 0 6 886.82 21.48
0 0 6 893.17 23.36
0 0 9 236.25 9.13
0 0 -9 220.33 9.28
0 0 -9 223.56 9.30
0 0 -12 4.09 3.91
0 0 12 15.29 4.31
0 0 -12 6.04 3.84
0 0 12 11.86 3.30
0 0 -12 12.21 4.15
0 0 -12 16.10 4.31
0 0 12 11.70 2.76
0 0 -12 9.05 3.00
0 0 15 13.75 3.89
0 0 -15 14.16 4.15
0 0 -15 14.08 5.17
0 0 15 21.40 4.85
0 0 -15 19.05 5.03
0 0 18 32.57 4.91
0 0 -18 37.09 4.80
0 0 18 35.32 5.15
0 0 -18 42.80 5.28
0 0 -18 29.92 4.80
1 0 -17 192.27 10.99
0 1 17 198.82 11.00
0 1 17 203.55 11.00
0 -1 -17 197.89 11.35
-1 0 17 196.58 10.69
-1 1 -17 200.22 10.46
0 -1 -17 208.51 10.39
-1 0 17 198.88 10.03
-1 1 -17 178.90 10.62
-1 0 17 213.49 11.08
1 0 -17 183.42 10.36
1 -1 17 192.29 10.61
-1 1 -14 430.08 17.28
-1 1 -14 391.80 17.49
0 -1 -14 376.52 16.89
0 1 14 417.76 17.20
0 -1 -14 381.98 17.80
0 -1 -14 381.85 16.70
1 0 -14 402.44 16.65
0 -1 -14 406.47 16.49
1 -1 14 397.89 17.17
1 0 -14 370.63 17.20
1 -1 14 416.50 15.83
-1 0 14 409.76 17.24
0 -1 -14 396.58 17.31
0 1 14 416.63 15.85
-1 0 14 412.77 16.58
1 0 -14 397.82 17.47
1 0 -11 -1.22 3.33
1 0 -11 1.07 2.73
-1 1 -11 3.04 3.67
0 -1 -11 -1.35 3.90
1 0 -11 2.26 3.52
1 -1 11 5.26 2.99
-1 1 -11 8.44 3.84
1 -1 11 -14.92 3.89
0 1 11 -0.97 2.61
-1 1 -11 -1.05 3.39
-1 0 11 4.00 3.15
0 -1 -11 7.30 2.96
-1 1 -11 -0.59 2.99
1 0 -11 -5.23 3.46
-1 0 11 1.49 3.33
0 -1 -11 -0.45 2.70
0 1 11 6.60 2.78
-1 0 11 3.13 2.70
0 -1 -11 1.23 3.45
0 -1 -11 1.01 2.59
1 -1 11 1.20 2.76
0 -1 -11 6.20 3.21
1 0 -11 1.89 2.84
0 1 11 1.27 3.37
1 0 -11 0.85 2.65
1 -1 11 4.12 2.04
-1 1 -11 6.95 2.58
1 0 -11 2.56 3.04
1 0 -8 10.75 2.75
1 0 -8 10.24 2.50
-1 1 -8 9.58 2.41
1 0 -8 10.69 2.30
1 -1 8 11.56 2.40
0 -1 -8 11.18 2.66
-1 0 8 10.75 2.51
-1 1 -8 8.34 2.37
-1 1 -8 11.61 2.30
0 1 8 9.29 2.17
0 -1 -8 8.79 2.59
1 -1 8 10.42 2.54
0 1 8 10.98 2.21
1 0 -5 1056.42 27.43
-1 1 -5 1041.16 26.97
-1 0 5 1029.03 26.24
1 -1 5 1032.12 26.38
0 -1 -5 1070.24 27.58
1 -1 5 1041.63 27.14
1 -1 5 1069.98 26.95
-1 0 5 1093.20 27.44
0 1 5 1091.46 27.02
-1 1 -5 1123.38 27.27
-1 1 -5 1138.00 27.10
1 -1 5 1100.35 27.45
1 0 -5 1134.84 28.06
0 1 5 1059.90 26.39
0 -1 -5 1090.23 27.59
0 1 5 1064.47 27.47
0 1 2 51.57 2.17
1 0 -2 53.55 1.59
1 -1 2 57.25 1.87
-1 1 -2 52.72 1.90
1 0 -2 56.10 2.65
0 -1 -2 50.35 2.33
-1 0 2 58.66 2.48
1 0 1 12.39 1.10
0 1 -1 14.02 0.98
-1 1 1 13.60 0.95
1 -1 -1 12.55 0.96
-1 0 -1 12.96 0.79
0 -1 1 16.35 1.04
-1 1 1 12.99 0.91
-1 0 -1 12.48 1.10
0 1 -4 216.05 6.68
1 0 4 215.94 6.77
1 0 4 209.28 6.45
-1 1 4 219.87 6.02
-1 0 -4 202.03 6.80
1 -1 -4 214.33 7.10
0 -1 4 212.83 6.67
-1 0 -4 230.93 7.05
0 -1 4 213.45 7.14
-1 1 4 210.84 6.46
-1 1 4 225.17 5.52
1 -1 -7 44.48 3.68
-1 0 -7 45.71 2.97
1 -1 -7 44.97 3.65
-1 0 -7 41.28 3.42
1 0 7 47.56 3.44
0 -1 7 43.58 3.25
0 1 -7 41.62 3.43
-1 0 -7 45.20 3.15
-1 1 7 41.19 3.62
0 1 -7 41.24 3.28
1 0 7 41.26 3.31
0 1 -7 42.53 3.33
-1 0 -10 13.18 3.59
0 1 -10 13.49 2.50
0 1 -10 10.97 2.85
1 -1 -10 11.07 3.36
1 -1 -10 14.97 4.09
-1 1 10 11.92 2.73
0 1 -10 9.67 3.60
1 0 10 9.75 2.31
-1 1 10 9.68 3.10
1 -1 -10 8.37 2.76
0 -1 10 15.95 2.87
1 -1 -10 8.68 3.14
0 1 -10 11.13 3.90
1 0 10 8.19 2.40
-1 0 -10 12.13 2.85
-1 0 -10 12.64 3.20
0 1 -10 10.64 2.73
1 -1 -13 32.13 4.85
-1 1 13 43.58 5.64
0 -1 13 40.48 4.83
-1 0 -13 28.92 5.16
-1 0 -13 37.65 6.11
-1 0 -13 32.51 4.93
1 0 13 36.65 5.63
0 1 -13 33.61 5.51
-1 1 13 46.44 5.11
1 -1 -13 46.80 5.69
0 1 -13 38.56 5.57
1 -1 -13 44.00 4.91
-1 1 13 38.52 4.94
1 0 13 43.77 5.34
1 -1 -13 31.85 5.50
-1 0 -13 37.60 5.28
1 -1 -13 37.63 6.00
0 -1 13 38.79 5.65
0 1 -13 34.52 5.97
-1 1 16 16.86 4.38
1 -1 -16 19.86 5.43
1 0 16 12.98 4.45
1 -1 -16 15.13 4.16
1 -1 -16 25.08 4.41
-1 1 16 21.32 4.31
-1 1 16 20.83 4.59
0 1 -16 17.79 5.02
0 -1 16 15.79 4.31
0 1 -16 11.84 4.40
-1 0 -16 16.26 5.30
0 -1 16 20.60 4.82
1 -1 -16 25.39 4.40
-1 0 -16 15.86 4.57
1 0 19 227.04 9.87
-1 1 19 232.93 9.40
0 -1 19 243.58 9.72
-1 0 -19 229.59 9.88
0 1 -19 212.01 9.62
1 -1 -19 233.12 10.15
-1 -1 18 17.15 3.35
-2 1 -18 25.18 4.67
2 -1 18 18.95 4.02
1 1 -18 21.34 4.52
-1 2 18 24.83 4.12
-1 -1 18 17.51 3.56
1 -2 -18 26.55 3.99
-2 1 -18 20.49 3.81
-1 -1 18 25.71 3.50
2 -1 18 23.36 3.60
-2 1 -18 20.08 4.17
1 -2 -18 26.25 4.66
1 1 -18 24.91 4.35
-1 2 15 149.05 8.83
-1 2 15 139.75 10.31
-1 -1 15 143.80 9.15
-1 -1 15 147.42 10.04
1 1 -15 159.65 9.74
1 1 -15 127.91 9.68
2 -1 15 133.34 9.60
-2 1 -15 152.20 9.79
1 -2 -15 146.21 9.87
1 -2 -15 158.18 10.48
1 -2 -15 134.76 9.63
-2 1 -15 129.43 10.04
2 -1 15 153.78 9.82
-1 2 15 158.46 10.28
1 1 -15 150.26 9.59
1 -2 -15 128.85 9.65
1 -2 -15 159.76 9.44
1 1 -12 354.76 15.12
-1 -1 12 345.09 14.46
-1 -1 12 335.49 14.90
1 1 -12 342.49 15.25
1 -2 -12 367.49 14.25
1 1 -12 339.36 15.04
-1 2 12 345.12 13.84
1 -2 -12 343.55 14.67
-2 1 -12 340.67 14.59
-1 2 12 362.36 14.50
2 -1 12 347.20 15.02
1 1 -12 352.97 14.10
2 -1 12 340.92 14.73
1 -2 -12 347.95 15.02
-2 1 -12 336.90 14.57
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1 1 -12 364.37 14.70
1 1 -12 354.78 15.38
1 -2 -12 325.82 14.81
-1 2 12 353.40 14.83
-1 -1 12 338.65 13.97
1 1 -12 335.97 14.54
1 -2 -12 330.81 13.81
1 1 -9 443.59 14.97
2 -1 9 453.89 15.11
-1 2 9 438.72 15.12
1 1 -9 435.69 14.51
-2 1 -9 453.42 14.26
1 -2 -9 441.35 15.37
1 1 -9 454.56 15.02
-2 1 -9 488.54 16.22
1 -2 -9 452.19 15.20
2 -1 9 460.68 14.38
-2 1 -9 434.19 14.76
1 1 -9 489.20 16.25
1 1 -9 488.41 16.35
1 -2 -9 439.37 15.40
-1 -1 9 454.30 14.94
1 -2 -6 1323.77 35.20
-1 2 6 1378.67 35.17
-2 1 -6 1347.50 34.46
-2 1 -6 1327.17 34.53
1 -2 -6 1370.98 35.28
2 -1 6 1443.99 35.80
1 1 -6 1347.68 35.64
-1 -1 6 1355.39 34.87
2 -1 6 1331.05 34.21
2 -1 6 1374.75 34.20
-1 2 6 1450.73 33.17
-1 -1 6 1351.47 33.89
-1 2 6 1322.70 34.07
2 -1 6 1358.73 34.98
1 1 -6 1328.14 34.77
2 -1 3 2848.88 63.92
-1 2 3 2557.24 62.78
-1 -1 3 2617.12 63.69
-1 2 3 2624.65 62.70
1 1 -3 2630.22 63.72
2 -1 3 2590.49 63.13
-1 -1 3 2665.97 63.34
-2 1 -3 2717.18 62.30
1 1 -3 2620.93 62.42
2 -1 3 2572.69 62.59
1 -2 -3 2599.30 63.36
1 -2 -3 2847.11 63.60
-1 -1 0 1928.90 47.02
1 -2 0 2084.71 47.11
-1 2 0 1914.01 46.99
1 1 0 1869.11 47.06
-2 1 0 1968.24 46.88
2 -1 0 1994.76 46.64
-2 1 0 1999.65 46.49
1 -2 3 1303.82 8.72
-1 -1 -3 1369.29 11.64
-1 2 -3 1296.04 7.48
2 -1 -3 1311.35 11.39
1 -2 3 1274.74 10.65
1 1 3 1313.77 10.33
1 -2 3 1281.05 11.51
-2 1 3 1342.08 9.78
1 -2 6 808.58 21.43
1 -2 6 819.96 22.20
-1 2 -6 794.73 22.04
-1 -1 -6 843.69 21.92
-1 2 -6 802.26 21.32
-2 1 6 839.39 20.85
-1 -1 -6 793.37 22.29
-1 2 -6 828.32 21.37
1 -2 6 809.67 22.13
-2 1 6 847.06 22.30
1 1 6 830.24 22.12
2 -1 -6 792.72 22.55
1 1 6 801.18 21.48
-2 1 9 47.96 4.22
-1 2 -9 45.96 4.14
2 -1 -9 52.57 4.61
-1 -1 -9 57.41 4.45
2 -1 -9 59.58 4.96
-1 2 -9 58.22 4.53
2 -1 -9 50.55 4.69
1 -2 9 60.45 4.13
-1 -1 -9 51.33 4.62
1 1 9 56.73 4.30
1 1 9 49.82 4.36
1 1 12 443.75 17.17
-1 2 -12 424.42 17.57
1 1 12 433.36 16.48
1 -2 12 445.13 16.67
-2 1 12 433.60 17.03
-1 2 -12 459.69 17.82
2 -1 -12 448.60 17.65
2 -1 -12 457.47 16.89
2 -1 -12 429.46 17.33
-1 2 -12 436.92 17.21
-1 -1 -12 454.31 17.35
1 -2 12 440.92 17.62
-2 1 12 471.87 17.13
-2 1 12 456.12 17.63
-1 -1 -12 436.46 17.42
2 -1 -12 445.46 17.81
2 -1 -12 448.62 17.24
2 -1 -12 439.82 17.28
-1 -1 -12 452.79 17.89
2 -1 -12 412.48 17.58
-1 -1 -12 401.32 17.33
1 1 12 441.70 17.43
-1 -1 -12 419.65 16.84
2 -1 -15 67.80 7.66
-2 1 15 77.94 7.78
-2 1 15 83.16 7.07
-2 1 15 64.04 7.20
-1 -1 -15 74.62 6.94
1 -2 15 80.67 6.68
-1 -1 -15 67.04 7.44
2 -1 -15 67.70 6.75
-1 -1 -15 66.00 7.68
-1 2 -15 68.67 7.33
1 -2 15 74.40 7.46
2 -1 -15 72.69 7.68
-2 1 15 82.99 6.85
-1 2 -15 76.76 7.42
2 -1 -15 66.58 7.89
1 1 15 71.84 7.04
-1 2 -18 166.23 8.82
1 -2 18 145.46 8.64
-2 1 18 161.61 8.21
-1 -1 -18 164.47 9.20
2 -1 -18 171.38 9.45
-1 2 -18 174.22 9.15
1 1 18 182.58 9.31
-2 1 18 155.55 8.45
-1 2 -18 144.96 8.79
1 1 18 181.91 9.04
1 -2 18 168.34 9.09
0 2 19 165.60 7.97
0 -2 -19 171.13 8.22
-2 2 -19 174.51 8.16
2 -2 19 165.34 7.86
2 0 -19 166.37 8.17
2 -2 16 69.52 7.05
-2 0 16 65.02 6.41
-2 0 16 72.37 6.43
-2 0 16 62.73 6.15
-2 2 -16 57.71 6.85
0 -2 -16 61.90 6.21
0 -2 -16 69.47 7.30
0 2 16 60.14 6.75
0 2 16 67.30 6.72
0 -2 -16 69.66 6.44
2 0 -16 66.83 6.61
2 0 -16 59.44 6.82
-2 2 -16 65.53 6.89
-2 0 16 71.55 7.52
2 0 -16 62.01 6.28
2 -2 13 239.07 10.84
2 0 -13 219.92 11.68
0 -2 -13 234.97 12.35
-2 2 -13 228.80 12.13
2 0 -13 234.21 11.93
-2 2 -13 228.58 12.45
2 0 -13 235.64 13.04
0 2 13 223.58 11.82
2 0 -13 245.86 12.63
-2 0 13 202.65 12.19
0 2 13 242.56 12.20
0 -2 -13 251.54 12.33
2 -2 13 233.56 11.97
2 -2 13 234.77 12.51
2 0 -13 230.55 12.34
0 -2 -13 213.67 12.36
0 -2 -13 249.20 11.79
0 -2 -13 206.26 12.11
2 0 -13 217.95 12.40
-2 0 13 220.28 11.76
2 0 -13 230.04 12.16
2 0 -10 160.93 8.84
2 0 -10 141.14 7.86
0 -2 -10 152.51 8.83
2 0 -10 145.19 8.18
-2 2 -10 159.85 8.84
0 -2 -10 150.10 8.76
2 0 -10 152.63 8.77
0 -2 -10 142.53 8.26
2 0 -10 162.01 8.87
0 2 10 174.72 8.65
0 2 10 152.79 7.96
-2 0 10 162.53 8.79
-2 0 10 161.58 8.50
-2 2 -10 151.37 8.46
-2 0 10 160.37 8.04
0 2 10 146.24 7.34
-2 2 -10 159.76 7.50
2 -2 10 148.18 8.16
0 -2 -10 161.02 8.04
0 2 7 552.54 16.73
-2 0 7 555.38 16.65
2 -2 7 547.04 15.64
2 0 -7 573.22 16.91
2 -2 7 528.21 17.00
2 0 -7 537.71 17.24
0 -2 -7 535.84 16.94
2 -2 7 576.99 16.78
-2 2 -7 536.41 16.31
0 2 7 587.73 15.42
0 2 7 553.40 15.94
2 -2 7 591.94 15.51
0 -2 -7 545.53 16.52
-2 2 -7 572.13 15.84
-2 0 7 583.79 15.36
2 -2 7 559.86 16.13
0 -2 -4 45.60 3.02
0 -2 -4 47.71 3.17
2 0 -4 38.94 3.38
0 -2 -4 48.98 3.18
-2 0 4 46.22 2.71
2 0 -4 41.10 1.31
0 2 4 42.46 2.87
2 0 -4 49.73 3.35
2 -2 4 44.51 2.06
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8 8 -3 184.51 8.23
-8 16 3 175.48 8.87
8 -16 0 210.77 9.65
8 -16 0 199.19 9.56
8 -16 0 201.79 9.22
-8 -8 0 191.73 8.35
-16 8 0 207.78 9.28
-8 -8 0 195.35 8.78
8 8 0 174.93 8.41
8 8 0 203.60 9.11
-8 16 0 211.17 9.53
8 -16 3 58.01 5.15
-8 -8 -3 64.51 4.38
-16 8 3 47.70 4.96
-8 -8 -3 53.69 4.65
8 8 3 56.14 4.89
-8 16 -3 44.45 4.75
7 -16 -4 0.18 2.08
-9 -7 4 2.78 1.58
-16 9 -4 -1.69 3.27
7 -16 -1 3.30 2.61
7 -16 -1 6.52 3.04
-16 9 -1 8.56 2.64
-9 -7 1 2.31 2.76
-16 9 -1 3.88 2.66
9 7 -1 2.05 2.66
-7 16 1 1.54 3.01
7 -16 2 6.87 3.01
7 -16 2 16.75 2.93
-9 -7 -2 9.56 2.59
-16 9 2 9.01 3.30
-9 -7 -2 7.88 2.80
9 7 2 16.42 2.98
9 7 2 9.53 2.71
-7 16 -2 11.79 3.61
6 -16 -2 0.84 2.56
-10 -6 2 -1.23 2.25
-16 10 -2 3.91 2.19
-16 10 -2 0.03 2.14
10 6 -2 0.56 2.07
-6 16 2 1.54 2.51
6 -16 1 42.36 4.39
6 -16 1 36.66 4.36
-10 -6 -1 30.92 3.60
-16 10 1 32.74 4.22
10 6 1 42.48 4.08
-6 16 -1 29.76 4.33
5 -16 0 100.45 6.19
11 5 0 100.18 6.03
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 50991
_shelx_res_file
;
kb11f.res created by SHELXL-2014/7
TITL kb11f in R-3, C18 H42 Fe N6 O6 3+, Cd2 Cl7 3-
CELL 1.54178 13.7143 13.7143 16.1312 90.000 90.000 120.000
ZERR 3.00 0.0001 0.0001 0.0002 0.000 0.000 0.000
LATT 3
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SFAC C H N O CL FE CD
UNIT 54 126 18 18 21 3 6
ACTA
TEMP -173
SIZE 0.062 0.05 0.045
CONF
REM Instructions for potential hydrogen bonds
EQIV $1 -x+4/3, -y+5/3, -z+2/3
HTAB C12 Cl2_$1
EQIV $2 -y+1, x-y+1, z
HTAB C1 Cl2_$2
HTAB C1 O1_$2
HTAB C12 Cl2_$2
BOND $H
L.S. 10
WGHT 0.042200 4.220000
FVAR 0.11567
CD1 7 0.333333 0.666667 0.323985 10.33333 0.01759 0.01759 =
0.01476 0.00000 0.00000 0.00879
FE1 6 0.333333 0.666667 0.666667 10.16667 0.01411 0.01411 =
0.01358 0.00000 0.00000 0.00706
O1 4 0.473672 0.754011 0.598897 11.00000 0.02069 0.02132 =
0.01831 0.00421 0.00510 0.01074
N1 3 0.595686 0.902502 0.520915 11.00000 0.02006 0.01949 =
0.01643 -0.00155 0.00140 0.00971
C1 1 0.494148 0.824776 0.542254 11.00000 0.02140 0.02105 =
0.01592 -0.00288 -0.00124 0.01141
H1 2 0.431130 0.818794 0.511126 11.00000 -1.20000
C11 1 0.696700 0.915050 0.560424 11.00000 0.02247 0.02609 =
0.02904 -0.00197 -0.00220 0.01256
AFIX 137
H113 2 0.739205 0.990196 0.585163 11.00000 -1.50000
H111 2 0.743491 0.905531 0.518941 11.00000 -1.50000
H112 2 0.675447 0.857876 0.603781 11.00000 -1.50000
AFIX 0
C12 1 0.612669 0.977171 0.451073 11.00000 0.02484 0.02668 =
0.02170 0.00361 0.00410 0.01294
AFIX 137
H123 2 0.654669 0.964516 0.407303 11.00000 -1.50000
H121 2 0.655312 1.055660 0.469591 11.00000 -1.50000
H122 2 0.539419 0.961434 0.429468 11.00000 -1.50000
AFIX 0
CL1 5 0.333333 0.666667 0.166667 10.16667 0.02997 0.02997 =
0.01001 0.00000 0.00000 0.01499
CL2 5 0.514277 0.692927 0.369511 11.00000 0.01913 0.02495 =
0.02008 -0.00203 -0.00193 0.01186
HKLF 4
REM kb11f in R-3, C18 H42 Fe N6 O6 3+, Cd2 Cl7 3-
REM R1 = 0.0196 for 980 Fo > 4sig(Fo) and 0.0221 for all 1051 data
REM 67 parameters refined using 0 restraints
END
WGHT 0.0248 7.7112
REM Highest difference peak 0.786, deepest hole -0.331, 1-sigma level 0.071
Q1 1 0.4910 0.8446 0.6411 11.00000 0.05 0.46
Q2 1 0.8228 0.9749 0.6193 11.00000 0.05 0.36
Q3 1 0.4992 0.7181 0.3218 11.00000 0.05 0.30
Q4 1 0.3333 0.6667 0.4986 10.33333 0.05 0.24
Q5 1 0.5668 0.8966 0.5479 11.00000 0.05 0.22
Q6 1 0.6686 0.7930 0.6470 11.00000 0.05 0.21
Q7 1 0.3333 0.6667 0.7520 10.33333 0.05 0.21
Q8 1 0.3316 0.8317 0.4785 11.00000 0.05 0.20
Q9 1 0.7640 0.9744 0.5342 11.00000 0.05 0.20
Q10 1 0.4911 0.7274 0.4273 11.00000 0.05 0.19
Q11 1 0.2406 0.7210 0.2678 11.00000 0.05 0.19
Q12 1 0.7159 1.0130 0.5700 11.00000 0.05 0.19
Q13 1 0.6290 0.9066 0.5390 11.00000 0.05 0.19
Q14 1 0.4248 0.6153 0.4022 11.00000 0.05 0.18
Q15 1 0.3333 0.6667 0.2620 10.33333 0.05 0.18
Q16 1 0.7472 0.9739 0.4030 11.00000 0.05 0.17
Q17 1 0.5124 0.6877 0.6070 11.00000 0.05 0.17
Q18 1 0.5651 0.7891 0.3815 11.00000 0.05 0.17
Q19 1 0.6338 1.0065 0.6098 11.00000 0.05 0.17
Q20 1 0.4317 0.7050 0.4750 11.00000 0.05 0.17
;
_shelx_res_checksum 40024
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_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 0.3333 0.6667 0.32398(2) 0.01664(12) Uani d 1 . .
Fe Fe1 0.3333 0.6667 0.6667 0.0139(2) Uani d 1 . .
O O1 0.47367(14) 0.75401(14) 0.59890(10) 0.0200(4) Uani d 1 . .
N N1 0.59569(16) 0.90250(17) 0.52091(12) 0.0187(4) Uani d 1 . .
C C1 0.4941(2) 0.8248(2) 0.54225(15) 0.0191(5) Uani d 1 . .
H H1 0.431(2) 0.819(2) 0.5111(17) 0.023 Uiso d 1 . .
C C11 0.6967(2) 0.9151(2) 0.56042(17) 0.0257(6) Uani d 1 . .
H H113 0.7392 0.9902 0.5852 0.039 Uiso calc 1 . .
H H111 0.7435 0.9055 0.5189 0.039 Uiso calc 1 . .
H H112 0.6754 0.8579 0.6038 0.039 Uiso calc 1 . .
C C12 0.6127(2) 0.9772(2) 0.45107(16) 0.0244(5) Uani d 1 . .
H H123 0.6547 0.9645 0.4073 0.037 Uiso calc 1 . .
H H121 0.6553 1.0557 0.4696 0.037 Uiso calc 1 . .
H H122 0.5394 0.9614 0.4295 0.037 Uiso calc 1 . .
Cl Cl1 0.3333 0.6667 0.1667 0.0233(3) Uani d 1 . .
Cl Cl2 0.51428(4) 0.69293(5) 0.36951(3) 0.02102(16) Uani 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 0.01759(14) 0.01759(14) 0.01476(17) 0.00879(7) 0.000 0.000
Fe1 0.0141(3) 0.0141(3) 0.0136(4) 0.00706(14) 0.000 0.000
O1 0.0207(8) 0.0213(8) 0.0183(8) 0.0107(7) 0.0051(6) 0.0042(7)
N1 0.0201(10) 0.0195(10) 0.0164(10) 0.0097(8) 0.0014(8) -0.0016(8)
C1 0.0214(12) 0.0210(12) 0.0159(11) 0.0114(10) -0.0012(9) -0.0029(10)
C11 0.0225(13) 0.0261(13) 0.0290(14) 0.0126(11) -0.0022(10) -0.0020(11)
C12 0.0248(13) 0.0267(13) 0.0217(13) 0.0129(11) 0.0041(10) 0.0036(10)
Cl1 0.0300(5) 0.0300(5) 0.0100(6) 0.0150(2) 0.000 0.000
Cl2 0.0191(3) 0.0249(3) 0.0201(3) 0.0119(2) -0.0019(2) -0.0020(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'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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'
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
Cl2 Cd1 Cl2 2_665 3_565 111.323(13) ?
Cl2 Cd1 Cl2 2_665 . 111.325(13) y
Cl2 Cd1 Cl2 3_565 . 111.324(13) ?
Cl2 Cd1 Cl1 2_665 . 107.547(14) ?
Cl2 Cd1 Cl1 3_565 . 107.549(14) ?
Cl2 Cd1 Cl1 . . 107.547(14) y
O1 Fe1 O1 14_456 3_565 86.85(7) ?
O1 Fe1 O1 14_456 2_665 180.0 ?
O1 Fe1 O1 3_565 2_665 93.16(7) ?
O1 Fe1 O1 3_565 . 93.15(7) y
O1 Fe1 O1 14_456 . 86.84(7) y
O1 Fe1 O1 2_665 . 93.15(7) ?
O1 Fe1 O1 14_456 13_566 93.16(7) ?
O1 Fe1 O1 3_565 13_566 86.85(7) ?
O1 Fe1 O1 2_665 13_566 86.84(7) ?
O1 Fe1 O1 . 13_566 180.0 ?
O1 Fe1 O1 14_456 15_556 93.16(7) ?
O1 Fe1 O1 3_565 15_556 180.00(8) ?
O1 Fe1 O1 2_665 15_556 86.84(7) ?
O1 Fe1 O1 . 15_556 86.85(7) ?
O1 Fe1 O1 13_566 15_556 93.15(7) ?
C1 O1 Fe1 . . 129.31(16) ?
C1 N1 C11 . . 123.0(2) ?
C1 N1 C12 . . 120.4(2) ?
C11 N1 C12 . . 116.51(19) ?
O1 C1 N1 . . 123.8(2) ?
O1 C1 H1 . . 117.8(17) ?
N1 C1 H1 . . 118.4(17) ?
N1 C11 H113 . . 109.5 ?
N1 C11 H111 . . 109.5 ?
H113 C11 H111 . . 109.5 ?
N1 C11 H112 . . 109.5 ?
H113 C11 H112 . . 109.5 ?
H111 C11 H112 . . 109.5 ?
N1 C12 H123 . . 109.5 ?
N1 C12 H121 . . 109.5 ?
H123 C12 H121 . . 109.5 ?
N1 C12 H122 . . 109.5 ?
H123 C12 H122 . . 109.5 ?
H121 C12 H122 . . 109.5 ?
Cd1 Cl1 Cd1 13_565 . 180.0 ?
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 Cl2 2_665 2.4358(5) ?
Cd1 Cl2 3_565 2.4358(5) ?
Cd1 Cl2 . 2.4358(5) y
Cd1 Cl1 . 2.5377(3) y
Fe1 O1 14_456 2.0071(16) ?
Fe1 O1 3_565 2.0072(16) ?
Fe1 O1 2_665 2.0072(16) ?
Fe1 O1 . 2.0072(16) y
Fe1 O1 13_566 2.0072(16) ?
Fe1 O1 15_556 2.0072(16) ?
O1 C1 . 1.258(3) ?
N1 C1 . 1.307(3) ?
N1 C11 . 1.455(3) ?
N1 C12 . 1.461(3) ?
C1 H1 . 0.97(3) ?
C11 H113 . 0.9800 ?
C11 H111 . 0.9800 ?
C11 H112 . 0.9800 ?
C12 H123 . 0.9800 ?
C12 H121 . 0.9800 ?
C12 H122 . 0.9800 ?
Cl1 Cd1 13_565 2.5376(3) ?
Cd1 Cd1 13_565 5.0752(3) ?
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
C12 H123 Cl2 16_665 0.98 2.82 3.783(3) 166.5
C1 H1 Cl2 2_665 0.97(3) 2.86(3) 3.772(3) 158(2)
C1 H1 O1 2_665 0.97(3) 2.62(3) 3.097(3) 111(2)
C12 H122 Cl2 2_665 0.98 2.94 3.861(3) 156.5
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
Fe1 O1 C1 N1 . . . . 156.61(17) ?
C11 N1 C1 O1 . . . . 0.4(4) ?
C12 N1 C1 O1 . . . . 176.2(2) ?
_cod_database_fobs_code 2243923