#------------------------------------------------------------------------------
#$Date: 2021-05-27 08:09:58 +0300 (Thu, 27 May 2021) $
#$Revision: 265535 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/23/2022382.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_2022382
loop_
_publ_author_name
'Sun, Yanwen'
'Chen, Zhen'
'Wang, Xiaozhong'
'Wang, Lei'
'Yang, Xue'
'Liang, Xiaoting'
'Fan, Shuangshuang'
'Zhang, Peiran'
_publ_section_title
;
Novel Ba^2+^ and Pb^2+^ metal--organic frameworks based on a semi-rigid
tetracarboxylic acid: syntheses, structures, topologies and luminescence
properties
;
_journal_coeditor_code DG3016
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229621005143
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac
'[Ba2 (C23 H20 O8) (C3 H7 N O) (H2 O)4], 3H2 O'
_chemical_formula_moiety 'C26 H35 Ba2 N O13, 3(H2 O1)'
_chemical_formula_sum 'C26 H41 Ba2 N O16'
_chemical_formula_weight 898.26
_chemical_name_systematic
'Poly[[di-\m-aqua-diaqua(dimethylformamide)[\m~7~-5,5'-methylenebis(2,4,6-trimethylbenzene-1,3-dicarboxylato)]dibarium(II)] trihydrate]'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_cell_angle_alpha 90
_cell_angle_beta 93.074(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 15.826(4)
_cell_length_b 13.033(3)
_cell_length_c 16.030(4)
_cell_measurement_reflns_used 9037
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.53
_cell_measurement_theta_min 2.36
_cell_volume 3301.6(14)
_computing_cell_refinement
;
APEX2 (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2005)
;
_computing_data_reduction
;
SAINT (Bruker, 2005)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Bruker APEXII CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0649
_diffrn_reflns_av_unetI/netI 0.0473
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 16023
_diffrn_reflns_theta_full 24.999
_diffrn_reflns_theta_max 24.999
_diffrn_reflns_theta_min 1.762
_exptl_absorpt_coefficient_mu 2.443
_exptl_absorpt_correction_T_max 0.7108
_exptl_absorpt_correction_T_min 0.6408
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2005)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.803
_exptl_crystal_description block
_exptl_crystal_F_000 1768
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.15
_refine_diff_density_max 1.265
_refine_diff_density_min -0.625
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 426
_refine_ls_number_reflns 5819
_refine_ls_number_restraints 619
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0382
_refine_ls_R_factor_gt 0.0315
_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^)+(0.0430P)^2^+1.1405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0790
_refine_ls_wR_factor_ref 0.0823
_reflns_number_gt 5034
_reflns_number_total 5819
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dg3016sup1.cif
_cod_data_source_block 1
_cod_original_cell_volume 3301.4(15)
_cod_database_code 2022382
_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 0.641
_shelx_estimated_absorpt_t_max 0.711
_shelx_hkl_file
;
0 0 3 0.54 0.31
0 0 4 4.90 0.63
0 0 4 6.21 0.91
0 0 5 0.10 0.40
0 0 5 -0.26 0.50
0 0 6 494.28 5.58
0 0 6 520.79 7.97
0 0 7 0.16 0.49
0 0 7 -0.10 0.79
0 0 8 1542.71 11.35
0 0 8 1494.36 15.65
0 0 9 1.34 0.69
0 0 9 0.53 0.89
0 0 10 52.58 2.46
0 0 10 55.21 3.61
0 0 11 1.09 1.31
0 0 12 206.95 7.47
0 0 13 -1.41 1.26
0 0 14 288.11 9.65
0 0 15 0.35 1.56
0 0 16 78.20 5.72
0 0 17 0.24 1.74
0 0 18 -0.40 1.79
0 0 19 -0.24 2.38
0 0 20 10.31 3.47
0 1 0 0.00 0.13
0 1 -1 0.27 0.20
0 1 1 0.38 0.22
0 1 -2 248.34 3.17
0 1 2 433.21 4.27
0 1 -3 3056.54 19.10
0 1 3 3114.79 19.51
0 1 3 3035.66 15.94
0 -1 4 107.11 2.83
0 1 -4 94.82 2.33
0 1 4 94.50 2.13
0 1 4 98.04 3.04
0 -1 5 603.69 7.47
0 1 -5 563.39 6.06
0 1 5 565.56 5.67
0 1 5 548.44 7.79
0 -1 6 1011.87 10.69
0 1 -6 917.25 8.29
0 1 6 946.81 7.95
0 1 6 884.36 10.76
0 -1 7 35.16 2.35
0 1 -7 35.58 1.91
0 1 7 32.53 1.70
0 1 7 29.17 2.36
0 -1 8 556.93 9.30
0 1 -8 535.81 6.98
0 1 8 528.49 6.54
0 1 8 504.97 9.39
0 -1 9 22.77 1.81
0 -1 9 29.60 2.51
0 1 9 23.85 1.74
0 1 9 28.92 2.78
0 -1 10 6.16 1.23
0 -1 10 6.95 1.73
0 1 10 7.50 1.17
0 1 10 7.79 1.82
0 -1 11 481.45 10.43
0 1 11 478.59 10.84
0 -1 12 4.66 1.72
0 1 12 3.81 1.67
0 -1 13 30.09 3.45
0 1 13 31.77 3.65
0 -1 14 59.68 4.56
0 1 14 63.32 4.85
0 -1 15 27.40 3.54
0 1 15 29.06 3.84
0 -1 16 111.85 6.71
0 1 16 113.66 7.00
0 -1 17 10.54 2.89
0 1 17 11.07 2.97
0 -1 18 16.79 3.64
0 1 18 18.02 3.70
0 -1 19 62.82 6.05
0 1 19 72.38 6.36
0 -1 20 56.98 5.98
0 1 20 59.99 6.04
0 2 0 62.26 1.92
0 2 -1 190.74 3.33
0 2 1 187.04 3.19
0 2 -2 163.72 3.21
0 2 2 164.78 3.04
0 -2 3 392.23 5.55
0 2 -3 28.63 1.45
0 2 3 443.88 5.13
0 2 3 406.85 5.75
0 -2 4 492.92 5.67
0 -2 4 445.40 6.52
0 2 -4 419.81 5.58
0 2 4 486.34 5.56
0 2 4 460.70 6.84
0 -2 5 403.33 5.83
0 2 -5 372.15 5.53
0 2 5 386.42 5.13
0 2 5 357.16 6.58
0 -2 6 631.70 8.10
0 2 -6 595.35 7.31
0 2 6 619.24 6.79
0 2 6 589.82 9.15
0 -2 7 30.64 2.16
0 2 -7 28.14 1.89
0 2 7 32.05 1.84
0 2 7 32.49 2.58
0 -2 8 40.70 2.63
0 2 -8 35.14 2.16
0 2 8 36.73 2.05
0 2 8 36.49 2.82
0 -2 9 396.59 8.19
0 2 -9 394.95 6.77
0 2 9 402.45 6.22
0 2 9 374.65 8.88
0 -2 10 410.47 8.88
0 2 -10 425.09 7.30
0 2 10 415.47 6.56
0 2 10 386.32 9.50
0 -2 11 13.85 2.12
0 2 11 16.63 2.64
0 -2 12 47.05 3.75
0 2 12 46.69 4.08
0 -2 13 48.39 3.98
0 2 13 51.01 4.30
0 -2 14 29.83 3.54
0 2 14 29.44 3.65
0 -2 15 39.66 4.07
0 2 15 34.84 4.00
0 -2 16 84.23 5.84
0 2 16 79.70 6.02
0 -2 17 293.53 10.71
0 2 17 274.09 10.97
0 -2 18 15.12 3.44
0 2 18 9.33 3.32
0 -2 19 2.95 2.60
0 2 19 4.35 3.03
0 2 20 16.33 4.10
0 -3 0 -0.11 0.49
0 3 0 0.24 0.54
0 -3 1 694.94 7.07
0 3 -1 721.93 7.78
0 3 1 713.48 7.57
0 -3 2 842.23 8.21
0 3 -2 843.30 8.59
0 3 2 870.56 8.40
0 3 2 722.68 7.33
0 -3 3 46.39 2.25
0 3 -3 46.08 2.25
0 3 3 47.50 2.15
0 3 3 42.57 2.11
0 -3 4 13.54 1.56
0 3 -4 14.32 1.55
0 3 4 17.36 1.45
0 3 4 14.34 1.51
0 -3 5 263.69 4.50
0 -3 5 236.17 5.48
0 3 -5 0.05 0.33
0 3 5 253.09 4.72
0 3 5 251.15 5.82
0 -3 6 795.21 8.75
0 -3 6 719.12 10.21
0 3 -6 728.94 8.98
0 3 6 771.94 8.42
0 3 6 689.73 10.25
0 -3 7 211.41 5.02
0 -3 7 195.05 5.79
0 3 -7 194.92 4.89
0 3 7 205.81 4.52
0 3 7 181.01 5.69
0 -3 8 4.32 1.24
0 3 -8 5.72 1.26
0 3 8 6.56 1.10
0 3 8 4.24 1.43
0 -3 9 447.61 8.44
0 3 -9 440.41 7.73
0 3 9 436.56 6.89
0 3 9 401.16 9.42
0 -3 10 67.95 3.72
0 3 -10 66.47 3.31
0 3 10 69.08 3.00
0 3 10 65.40 4.18
0 -3 11 74.38 4.12
0 3 -11 72.51 3.58
0 3 11 67.10 4.46
0 -3 12 82.51 4.59
0 3 12 75.91 5.00
0 -3 13 404.27 10.20
0 3 13 382.48 11.16
0 -3 14 59.88 4.56
0 3 14 65.62 5.12
0 -3 15 18.54 3.04
0 3 15 21.99 3.49
0 -3 16 1.73 2.04
0 3 16 3.71 2.42
0 -3 17 22.50 3.58
0 3 17 23.28 3.94
0 -3 18 32.90 4.66
0 3 18 22.35 4.18
0 -3 19 1.63 2.36
0 3 19 -0.39 1.94
0 -3 20 29.55 4.86
0 3 20 26.97 4.77
0 -4 0 1.82 0.76
0 4 0 2.65 0.84
0 -4 1 173.87 4.09
0 4 -1 177.57 4.47
0 4 1 184.50 4.49
0 4 1 153.16 3.25
0 -4 2 1150.26 10.67
0 4 -2 1155.06 11.44
0 4 2 1205.65 11.33
0 -4 3 48.54 2.51
0 4 -3 46.84 2.60
0 4 3 45.19 2.44
0 4 3 42.45 2.29
0 -4 4 149.28 4.39
0 4 -4 148.93 4.37
0 4 4 158.78 4.23
0 4 4 152.24 4.44
0 -4 5 174.37 3.51
0 -4 5 159.11 4.83
0 4 -5 166.42 4.71
0 4 5 172.29 4.46
0 4 5 157.41 4.83
0 -4 6 95.29 3.00
0 -4 6 91.04 3.97
0 4 -6 87.92 3.61
0 4 6 96.83 3.47
0 4 6 83.56 3.86
0 -4 7 684.64 8.59
0 -4 7 630.47 10.55
0 4 7 651.41 8.74
0 4 7 596.82 10.54
0 -4 8 -0.01 0.78
0 -4 8 1.16 1.02
0 4 -8 0.59 0.84
0 4 8 1.16 0.81
0 4 8 1.53 1.13
0 -4 9 5.87 1.29
0 -4 9 3.39 1.44
0 4 -9 2.81 1.13
0 4 9 4.10 1.13
0 4 9 4.85 1.57
0 -4 10 73.60 3.76
0 -4 10 64.11 4.25
0 4 -10 69.47 3.63
0 4 10 76.62 3.36
0 4 10 67.81 4.47
0 -4 11 45.51 3.31
0 -4 11 42.83 3.85
0 4 -11 40.75 3.09
0 4 11 36.56 3.55
0 -4 12 183.63 6.49
0 -4 12 183.14 7.59
0 4 12 168.41 7.45
0 -4 13 9.21 2.23
0 -4 13 12.73 2.60
0 4 13 10.43 2.54
0 -4 14 5.67 2.12
0 -4 14 9.58 2.58
0 4 14 7.65 2.51
0 -4 15 375.50 12.07
0 4 15 310.31 11.17
0 -4 16 53.18 5.23
0 4 16 45.00 4.87
0 -4 17 1.80 2.07
0 4 17 0.43 1.98
0 -4 18 8.89 3.03
0 4 18 4.21 2.72
0 -4 19 52.23 5.79
0 4 19 36.61 5.08
0 -4 20 14.76 3.90
0 4 20 8.80 3.59
0 -5 0 -0.16 0.72
0 5 0 1.39 0.87
0 -5 1 522.08 7.75
0 5 -1 518.57 8.42
0 5 1 508.69 8.21
0 5 1 444.63 5.91
0 -5 2 5.14 1.09
0 5 -2 3.83 1.10
0 5 2 6.28 1.22
0 5 2 5.02 0.97
0 -5 3 42.64 2.61
0 5 -3 40.95 2.74
0 5 3 47.87 2.76
0 5 3 30.70 2.02
0 -5 4 2088.05 17.10
0 5 -4 2043.12 17.45
0 5 4 2173.59 17.10
0 5 4 1904.64 16.10
0 -5 5 23.88 2.31
0 5 -5 28.14 2.42
0 5 5 29.81 2.41
0 5 5 25.48 2.39
0 -5 6 69.75 2.46
0 -5 6 63.41 3.58
0 5 -6 63.06 3.39
0 5 6 67.93 3.25
0 5 6 61.75 3.48
0 -5 7 154.15 3.98
0 -5 7 148.48 5.46
0 5 -7 143.45 5.02
0 5 7 157.57 4.84
0 5 7 141.55 5.41
0 -5 8 167.36 4.56
0 -5 8 143.58 5.66
0 5 -8 59.70 3.34
0 5 8 165.29 5.01
0 5 8 145.11 5.83
0 -5 9 23.08 2.22
0 -5 9 34.64 3.20
0 5 -9 23.62 2.51
0 5 9 29.42 2.48
0 5 9 32.57 3.35
0 -5 10 195.20 5.76
0 -5 10 190.34 7.18
0 5 -10 199.03 6.34
0 5 10 198.83 5.67
0 5 10 177.76 7.07
0 -5 11 18.21 2.30
0 -5 11 17.67 2.77
0 5 -11 16.52 2.36
0 5 11 15.87 2.72
0 -5 12 402.90 11.22
0 5 12 362.29 10.89
0 -5 13 1.97 1.66
0 5 13 0.28 1.73
0 -5 14 0.85 1.65
0 5 14 1.56 1.77
0 -5 15 -0.74 1.44
0 5 15 -0.80 1.62
0 -5 16 53.67 5.19
0 5 16 46.56 4.99
0 -5 17 1.24 2.04
0 5 17 0.06 2.12
0 -5 18 200.52 10.19
0 5 18 174.87 9.63
0 -5 19 8.27 3.25
0 5 19 5.51 3.12
0 6 0 146.33 4.98
0 6 0 122.21 3.04
0 -6 1 529.60 8.61
0 6 -1 473.27 8.82
0 6 1 495.74 8.94
0 6 1 430.04 6.22
0 -6 2 592.54 9.18
0 6 -2 590.17 9.96
0 6 2 597.67 9.78
0 6 2 517.28 7.49
0 -6 3 206.34 5.65
0 6 -3 199.61 5.98
0 6 3 203.86 5.80
0 6 3 110.07 3.83
0 -6 4 50.40 3.11
0 6 -4 46.36 3.16
0 6 4 55.51 3.26
0 6 4 50.16 2.96
0 -6 5 10.57 1.68
0 6 -5 8.23 1.66
0 6 5 9.79 1.65
0 6 5 9.34 1.62
0 -6 6 26.70 1.58
0 -6 6 27.10 2.63
0 6 -6 28.75 2.68
0 6 6 28.08 2.51
0 6 6 25.14 2.48
0 -6 7 138.48 5.50
0 6 -7 142.03 5.41
0 6 7 144.74 5.08
0 6 7 130.76 5.41
0 -6 8 14.29 2.26
0 6 -8 11.11 1.96
0 6 8 12.68 1.96
0 6 8 17.23 2.40
0 -6 9 264.72 8.25
0 6 -9 234.91 7.13
0 6 9 261.24 6.87
0 6 9 225.49 7.76
0 -6 10 324.17 9.47
0 6 -10 0.84 0.85
0 6 10 333.48 7.81
0 6 10 296.62 9.29
0 -6 11 127.44 6.44
0 6 -11 131.51 5.69
0 6 11 117.83 6.38
0 -6 12 160.78 7.42
0 6 12 163.10 7.70
0 -6 13 2.36 1.71
0 6 13 2.61 2.04
0 -6 14 15.52 3.02
0 6 14 13.62 3.08
0 -6 15 105.84 6.89
0 6 15 96.31 6.85
0 -6 16 11.31 3.08
0 6 16 5.91 2.70
0 -6 17 53.31 5.64
0 6 17 40.68 5.06
0 -6 18 5.53 2.76
0 6 18 5.64 3.04
0 -6 19 9.23 3.42
0 6 19 7.57 3.34
0 7 0 -0.86 0.85
0 7 0 -0.88 0.53
0 -7 1 216.88 6.08
0 7 -1 223.29 6.69
0 7 1 214.52 6.49
0 7 1 181.07 4.34
0 -7 2 557.24 9.62
0 7 -2 549.17 10.40
0 7 2 558.71 10.28
0 7 2 504.46 7.81
0 -7 3 4.87 1.33
0 7 -3 6.11 1.53
0 7 3 5.59 1.45
0 7 3 4.63 1.16
0 -7 4 96.22 4.36
0 7 -4 97.50 4.65
0 7 4 92.11 4.35
0 -7 5 97.81 4.58
0 7 -5 99.08 4.76
0 7 5 102.31 4.65
0 7 5 99.12 4.44
0 -7 6 613.68 11.30
0 7 -6 590.35 11.34
0 7 6 613.53 10.89
0 7 6 573.27 10.84
0 -7 7 26.15 2.91
0 7 -7 22.86 2.81
0 7 7 28.38 2.85
0 7 7 23.81 2.92
0 -7 8 32.22 3.32
0 7 -8 33.20 3.25
0 7 8 36.64 3.18
0 7 8 29.36 3.15
0 -7 9 90.30 5.22
0 7 -9 91.97 4.96
0 7 9 89.56 4.57
0 7 9 87.66 5.29
0 -7 10 1.12 1.59
0 7 -10 4.04 1.64
0 7 10 0.99 1.43
0 7 10 3.03 1.72
0 -7 11 11.01 2.52
0 7 -11 1.57 1.16
0 7 11 11.53 2.65
0 -7 12 7.27 2.32
0 7 12 8.42 2.52
0 -7 13 153.89 7.73
0 7 13 145.88 7.71
0 -7 14 192.10 8.91
0 7 14 180.04 8.83
0 -7 15 3.83 2.21
0 7 15 3.25 2.42
0 -7 16 44.38 5.16
0 7 16 36.99 4.92
0 -7 17 12.40 3.43
0 7 17 13.29 3.65
0 -7 18 -1.08 2.08
0 7 18 1.89 2.61
0 8 0 113.47 5.20
0 8 0 97.99 3.15
0 -8 1 22.14 2.53
0 8 -1 22.60 2.71
0 8 1 23.21 2.76
0 8 1 23.03 1.94
0 -8 2 114.21 4.89
0 8 -2 118.00 5.37
0 8 2 114.94 5.20
0 8 2 99.12 3.78
0 -8 3 248.47 7.12
0 8 -3 237.56 7.52
0 8 3 241.78 7.38
0 8 3 217.87 5.89
0 -8 4 25.92 2.86
0 8 -4 24.40 2.97
0 8 4 25.17 2.87
0 8 4 20.79 2.41
0 -8 5 775.35 12.91
0 8 -5 782.83 13.74
0 8 5 802.39 13.28
0 8 5 716.33 11.84
0 -8 6 63.70 4.19
0 8 -6 60.55 4.13
0 8 6 67.40 4.16
0 8 6 55.04 3.71
0 -8 7 27.35 3.14
0 8 -7 24.95 2.96
0 8 7 27.17 3.00
0 8 7 28.09 3.09
0 -8 8 249.82 8.26
0 8 -8 254.31 8.24
0 8 8 255.36 7.77
0 8 8 245.51 8.24
0 -8 9 77.43 5.01
0 8 -9 77.83 4.85
0 8 9 82.08 4.67
0 8 9 73.09 4.89
0 -8 10 17.02 2.85
0 8 -10 17.60 2.81
0 8 10 17.33 2.93
0 -8 11 13.84 2.71
0 8 -11 8.91 2.30
0 8 11 6.93 2.45
0 -8 12 2.41 1.95
0 8 12 1.97 2.08
0 -8 13 47.37 4.88
0 8 13 38.78 4.68
0 -8 14 107.18 7.03
0 8 14 91.21 6.60
0 -8 15 0.34 1.79
0 8 15 1.97 2.27
0 -8 16 69.43 6.25
0 8 16 52.71 5.91
0 -8 17 159.32 9.28
0 8 17 124.84 8.53
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10 -2 6 316.51 8.96
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10 2 6 323.33 8.00
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10 -2 7 409.54 10.52
10 2 7 359.53 10.38
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10 -2 8 191.79 7.67
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10 -2 9 2.90 1.87
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10 -2 12 2.17 1.82
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10 3 11 217.24 8.61
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0 0 0 0.00 0.00
;
_shelx_hkl_checksum 48214
_shelx_res_file
;
TITL p in P2(1)/n
p.res
created by SHELXL-2017/1 at 16:16:00 on 19-May-2021
CELL 0.71073 15.8257 13.0326 16.0299 90 93.074 90
ZERR 4 0.0041 0.0033 0.004 0 0.004 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H O Ba N
UNIT 104 164 64 8 4
EQIV $1 0.5+X,1.5-Y,0.5+Z
EQIV $2 -X,1-Y,-Z
EQIV $3 0.5-X,-0.5+Y,0.5-Z
EQIV $4 0.5+X,0.5-Y,-0.5+Z
DELU 0.01 0.02 O9 C24
SIMU 0.01 0.02 3.8 C15 C3 C13 C2 C16 C9 C8 C4 C5 C1 C12 C7 C11 C20 C23 C10 =
C6 C22 C17 C18 C19 C21 C14 C24 C25 C26 O9
L.S. 4
PLAN 20
SIZE 0.2 0.2 0.15
TEMP 0
HTAB O3W O6W
HTAB O4W O7W
HTAB O5W O6W
HTAB O5W O7W
HTAB C26 O8_$1
HTAB O3W O5_$2
HTAB O4W O3_$3
HTAB O6W O6_$4
HTAB O6W O8_$2
HTAB O1W O5_$2
HTAB O1W O4_$4
BOND $H
htab
fmap 2
acta
OMIT -3 50
OMIT 0 2 0
OMIT 1 0 7
OMIT 1 1 4
OMIT -1 0 3
OMIT 3 1 5
OMIT -2 2 2
REM
REM
REM
WGHT 0.043000 1.140500
FVAR 0.14707
BA1 4 0.497996 0.451004 0.186815 11.00000 0.01685 0.02292 =
0.02587 0.00247 0.00089 -0.00069
BA2 4 0.439057 0.163813 0.045454 11.00000 0.02899 0.02361 =
0.02588 0.00129 0.00718 0.00047
O5 3 -0.349680 0.548921 0.111449 11.00000 0.02121 0.05328 =
0.05305 0.01298 -0.01267 0.00064
O1W 3 0.461921 0.385916 0.023729 11.00000 0.03417 0.03546 =
0.02540 -0.00071 0.00620 0.00466
O8 3 -0.041037 0.799267 0.198567 11.00000 0.03941 0.02857 =
0.03847 -0.00259 0.00019 -0.00567
C15 1 0.064509 0.226203 0.373322 11.00000 0.01529 0.02918 =
0.02269 0.00048 0.00198 -0.00040
O4 3 0.056003 0.132397 0.384891 11.00000 0.03647 0.02189 =
0.03146 0.00064 0.00720 -0.00518
C3 1 0.093122 0.265351 0.290309 11.00000 0.01916 0.02287 =
0.02177 -0.00229 0.00528 0.00104
O3 3 0.050707 0.294107 0.426779 11.00000 0.04228 0.02966 =
0.02904 -0.00395 0.01430 -0.00325
C13 1 -0.034124 0.561632 0.168660 11.00000 0.01517 0.02623 =
0.02487 0.00358 -0.00058 0.00206
C2 1 0.179042 0.268704 0.276888 11.00000 0.01777 0.03030 =
0.02481 0.00033 0.00351 0.00080
C16 1 -0.301961 0.506343 0.164249 11.00000 0.01646 0.03013 =
0.03822 -0.00099 -0.00202 -0.00012
C9 1 -0.155682 0.459036 0.123354 11.00000 0.01632 0.02503 =
0.02279 0.00238 -0.00235 -0.00110
C8 1 -0.067618 0.473279 0.129725 11.00000 0.01655 0.02424 =
0.02220 0.00043 0.00091 0.00183
C4 1 0.032557 0.303170 0.231841 11.00000 0.01538 0.02564 =
0.02396 -0.00182 0.00515 -0.00093
C5 1 0.057986 0.348496 0.157538 11.00000 0.01811 0.02528 =
0.02423 -0.00068 0.00394 0.00031
C1 1 0.204009 0.310248 0.201966 11.00000 0.01686 0.03211 =
0.02725 0.00175 0.00642 0.00429
C12 1 -0.087680 0.628582 0.209935 11.00000 0.01871 0.02457 =
0.02759 -0.00182 -0.00214 0.00105
C7 1 -0.007569 0.394583 0.094761 11.00000 0.01865 0.03014 =
0.02328 -0.00204 0.00243 0.00165
AFIX 23
H7A 2 0.022185 0.426883 0.050383 11.00000 -1.20000
H7B 2 -0.041113 0.339076 0.069930 11.00000 -1.20000
AFIX 0
O6 3 -0.328577 0.446217 0.218266 11.00000 0.02089 0.08244 =
0.07857 0.04206 0.00057 -0.01208
C11 1 -0.174197 0.607660 0.213366 11.00000 0.01600 0.02837 =
0.02719 0.00239 0.00231 0.00185
C20 1 0.178143 0.392131 0.062044 11.00000 0.02786 0.05387 =
0.03744 0.01097 0.01567 0.00665
AFIX 137
H20A 2 0.142686 0.369015 0.015316 11.00000 -1.50000
H20B 2 0.234972 0.368557 0.056076 11.00000 -1.50000
H20C 2 0.177592 0.465749 0.064013 11.00000 -1.50000
AFIX 0
C23 1 -0.196714 0.373713 0.071719 11.00000 0.02224 0.03138 =
0.03962 -0.00586 -0.00484 -0.00058
AFIX 137
H23A 2 -0.173443 0.372385 0.017641 11.00000 -1.50000
H23B 2 -0.256616 0.385373 0.065483 11.00000 -1.50000
H23C 2 -0.186137 0.309203 0.099243 11.00000 -1.50000
AFIX 0
C10 1 -0.207078 0.526014 0.166225 11.00000 0.01357 0.02659 =
0.02846 0.00340 0.00130 -0.00031
C6 1 0.145389 0.349771 0.141843 11.00000 0.01682 0.02809 =
0.02373 0.00141 0.00470 0.00367
C22 1 -0.229818 0.673459 0.265397 11.00000 0.02165 0.04445 =
0.04690 -0.00902 0.00494 0.00593
AFIX 137
H22A 2 -0.227242 0.648712 0.321884 11.00000 -1.50000
H22B 2 -0.287159 0.670245 0.242760 11.00000 -1.50000
H22C 2 -0.210380 0.743211 0.264595 11.00000 -1.50000
AFIX 0
O1 3 0.336123 0.394511 0.208203 11.00000 0.02385 0.09084 =
0.08403 0.02698 0.00433 -0.01656
C17 1 -0.052045 0.726953 0.248291 11.00000 0.01287 0.03111 =
0.03325 -0.00443 -0.00294 0.00329
C18 1 0.242967 0.231094 0.343086 11.00000 0.02491 0.07235 =
0.03479 0.01400 0.00305 0.01154
AFIX 137
H18A 2 0.226643 0.253227 0.397029 11.00000 -1.50000
H18B 2 0.297676 0.258606 0.332662 11.00000 -1.50000
H18C 2 0.245274 0.157509 0.341705 11.00000 -1.50000
AFIX 0
C19 1 -0.059594 0.293153 0.250514 11.00000 0.01793 0.04012 =
0.03300 0.00952 0.00312 -0.00111
AFIX 137
H19A 2 -0.066126 0.238515 0.289815 11.00000 -1.50000
H19B 2 -0.092365 0.278275 0.199824 11.00000 -1.50000
H19C 2 -0.078875 0.356300 0.273773 11.00000 -1.50000
AFIX 0
C21 1 0.058058 0.588595 0.166384 11.00000 0.01847 0.03027 =
0.04282 -0.00359 0.00420 -0.00107
AFIX 137
H21A 2 0.091063 0.540314 0.199549 11.00000 -1.50000
H21B 2 0.067175 0.656430 0.188410 11.00000 -1.50000
H21C 2 0.074817 0.586262 0.109739 11.00000 -1.50000
AFIX 0
O2 3 0.329360 0.239389 0.153154 11.00000 0.03772 0.12796 =
0.04802 -0.00175 0.01422 0.04532
C14 1 0.296999 0.314630 0.185989 11.00000 0.02037 0.06010 =
0.03143 0.01289 0.00483 0.00490
O7 3 -0.036881 0.732559 0.324955 11.00000 0.03359 0.03842 =
0.02947 -0.00531 -0.00665 -0.00152
N1 5 0.526869 0.621964 0.457300 11.00000 0.08692 0.05141 =
0.04441 -0.00385 0.01267 -0.00519
O9 3 0.508240 0.556624 0.329383 11.00000 0.15919 0.05715 =
0.04322 -0.01164 -0.01407 0.00700
C24 1 0.554057 0.585792 0.389625 11.00000 0.14998 0.05507 =
0.05556 0.00675 0.01318 0.00486
AFIX 43
H24 2 0.612314 0.581101 0.385432 11.00000 -1.20000
AFIX 0
C25 1 0.438501 0.635833 0.469646 11.00000 0.12366 0.08768 =
0.12678 0.03074 0.04764 0.00313
AFIX 137
H25A 2 0.406182 0.618260 0.419280 11.00000 -1.50000
H25B 2 0.428086 0.706177 0.483597 11.00000 -1.50000
H25C 2 0.422090 0.592343 0.514325 11.00000 -1.50000
AFIX 0
C26 1 0.577478 0.648213 0.528583 11.00000 0.19755 0.07974 =
0.07331 0.00830 -0.02877 -0.02181
AFIX 137
H26A 2 0.628675 0.608593 0.530060 11.00000 -1.50000
H26B 2 0.547276 0.634093 0.577662 11.00000 -1.50000
H26C 2 0.591134 0.719925 0.526831 11.00000 -1.50000
AFIX 0
O3W 3 0.324929 0.246534 -0.065731 11.00000 0.04409 0.05221 =
0.05376 0.00395 -0.01483 -0.00511
AFIX 3
H3WA 2 0.326639 0.307674 -0.084021 11.00000 -1.20000
H3WB 2 0.281939 0.216674 -0.088641 11.00000 -1.20000
AFIX 0
O2W 3 0.579376 0.015847 0.072429 11.00000 0.04990 0.05982 =
0.05998 -0.01363 -0.00078 0.01134
O4W 3 0.412620 -0.010222 0.133171 11.00000 0.09334 0.03749 =
0.07001 0.00770 0.03613 -0.00005
AFIX 3
H4WA 2 0.420490 -0.070662 0.115231 11.00000 -1.20000
H4WB 2 0.360920 -0.004082 0.144181 11.00000 -1.20000
AFIX 0
O5W 3 0.272426 0.018627 -0.000638 11.00000 0.08433 0.27966 =
0.12377 0.08358 0.02482 0.06933
AFIX 7
H5WA 2 0.235027 0.043686 -0.035199 11.00000 -1.20000
H5WB 2 0.243046 0.002587 0.040552 11.00000 -1.20000
AFIX 0
O6W 3 0.192319 0.126369 -0.126893 11.00000 0.05567 0.08730 =
0.05806 0.00240 -0.01221 -0.00524
AFIX 3
H6WA 2 0.196549 0.102619 -0.175873 11.00000 -1.20000
H6WB 2 0.142909 0.147869 -0.117973 11.00000 -1.20000
AFIX 6
O7W 3 0.239052 0.024811 0.174102 11.00000 0.07748 0.07019 =
0.11118 -0.00411 0.01169 0.00020
H7WA 2 0.239996 0.084981 0.194632 11.00000 -1.50000
H7WB 2 0.212761 -0.015072 0.205710 11.00000 -1.50000
AFIX 0
H1WA 2 0.498119 0.386057 -0.006400 11.00000 0.02693
H1WB 2 0.414255 0.415028 0.003343 11.00000 0.08504
HKLF 4
REM p in P2(1)/n
REM R1 = 0.0315 for 5034 Fo > 4sig(Fo) and 0.0382 for all 5819 data
REM 426 parameters refined using 619 restraints
END
WGHT 0.0430 1.1405
REM Instructions for potential hydrogen bonds
HTAB C26 O8_$1
HTAB O3W O5_$2
HTAB O3W O6W
HTAB O4W O3_$3
HTAB O4W O7W
HTAB O5W O6W
HTAB O5W O7W
HTAB O6W O6_$4
HTAB O6W O8_$2
HTAB O1W O4_$4
HTAB O1W O5_$2
REM Highest difference peak 1.265, deepest hole -0.625, 1-sigma level 0.122
Q1 1 0.4972 0.5235 0.1861 11.00000 0.05 1.27
Q2 1 0.4401 0.2398 0.0454 11.00000 0.05 1.22
Q3 1 0.4982 0.3817 0.1857 11.00000 0.05 1.05
Q4 1 0.4406 0.0889 0.0451 11.00000 0.05 1.03
Q5 1 0.4659 0.6008 0.3824 11.00000 0.05 0.85
Q6 1 0.2617 0.0588 -0.1291 11.00000 0.05 0.83
Q7 1 0.6130 0.6160 0.4615 11.00000 0.05 0.82
Q8 1 0.3584 -0.0111 0.0900 11.00000 0.05 0.76
Q9 1 0.4959 0.6613 0.5270 11.00000 0.05 0.70
Q10 1 0.2807 0.0392 0.0046 11.00000 0.05 0.69
Q11 1 0.4813 0.1531 0.0787 11.00000 0.05 0.50
Q12 1 0.1430 0.4378 0.0289 11.00000 0.05 0.46
Q13 1 0.4491 0.3019 0.0014 11.00000 0.05 0.45
Q14 1 -0.0648 0.6004 0.1751 11.00000 0.05 0.44
Q15 1 0.3429 0.2161 0.1719 11.00000 0.05 0.44
Q16 1 -0.2517 0.7349 0.2339 11.00000 0.05 0.41
Q17 1 0.4590 0.1273 0.0888 11.00000 0.05 0.41
Q18 1 0.4365 0.5380 0.3241 11.00000 0.05 0.41
Q19 1 -0.0152 0.6625 0.3391 11.00000 0.05 0.40
Q20 1 0.3398 0.3067 0.1257 11.00000 0.05 0.40
;
_shelx_res_checksum 9483
loop_
_space_group_symop_operation_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_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
Ba Ba1 0.49800(2) 0.45100(2) 0.18681(2) 0.02189(9) Uani d 1 . .
Ba Ba2 0.43906(2) 0.16381(2) 0.04545(2) 0.02595(9) Uani d 1 . .
O O5 -0.34968(19) 0.5489(3) 0.1114(2) 0.0430(8) Uani d 1 . .
O O1W 0.4619(2) 0.3859(2) 0.02373(19) 0.0315(7) Uani d 1 . .
O O8 -0.0410(2) 0.7993(2) 0.19857(19) 0.0356(7) Uani d 1 . .
C C15 0.0645(2) 0.2262(3) 0.3733(2) 0.0224(8) Uani d 1 . .
O O4 0.05600(18) 0.1324(2) 0.38489(17) 0.0297(6) Uani d 1 . .
C C3 0.0931(2) 0.2654(3) 0.2903(2) 0.0211(8) Uani d 1 . .
O O3 0.05071(19) 0.2941(2) 0.42678(18) 0.0332(7) Uani d 1 . .
C C13 -0.0341(2) 0.5616(3) 0.1687(2) 0.0221(8) Uani d 1 . .
C C2 0.1790(2) 0.2687(3) 0.2769(2) 0.0242(8) Uani d 1 . .
C C16 -0.3020(2) 0.5063(3) 0.1642(3) 0.0284(9) Uani d 1 . .
C C9 -0.1557(2) 0.4590(3) 0.1234(2) 0.0215(8) Uani d 1 . .
C C8 -0.0676(2) 0.4733(3) 0.1297(2) 0.0210(7) Uani d 1 . .
C C4 0.0326(2) 0.3032(3) 0.2318(2) 0.0215(7) Uani d 1 . .
C C5 0.0580(2) 0.3485(3) 0.1575(2) 0.0224(8) Uani d 1 . .
C C1 0.2040(2) 0.3102(3) 0.2020(3) 0.0252(8) Uani d 1 . .
C C12 -0.0877(2) 0.6286(3) 0.2099(2) 0.0237(8) Uani d 1 . .
C C7 -0.0076(2) 0.3946(3) 0.0948(2) 0.0240(8) Uani d 1 . .
H H7A 0.022185 0.426883 0.050383 0.029 Uiso calc 1 . .
H H7B -0.041113 0.339076 0.069930 0.029 Uiso calc 1 . .
O O6 -0.3286(2) 0.4462(3) 0.2183(3) 0.0607(11) Uani d 1 . .
C C11 -0.1742(2) 0.6077(3) 0.2134(2) 0.0238(8) Uani d 1 . .
C C20 0.1781(3) 0.3921(4) 0.0620(3) 0.0392(11) Uani d 1 . .
H H20A 0.142686 0.369015 0.015317 0.059 Uiso calc 1 . .
H H20B 0.234971 0.368557 0.056076 0.059 Uiso calc 1 . .
H H20C 0.177592 0.465749 0.064013 0.059 Uiso calc 1 . .
C C23 -0.1967(3) 0.3737(3) 0.0717(3) 0.0313(9) Uani d 1 . .
H H23A -0.173443 0.372385 0.017641 0.047 Uiso calc 1 . .
H H23B -0.256616 0.385373 0.065483 0.047 Uiso calc 1 . .
H H23C -0.186137 0.309203 0.099243 0.047 Uiso calc 1 . .
C C10 -0.2071(2) 0.5260(3) 0.1662(2) 0.0229(8) Uani d 1 . .
C C6 0.1454(2) 0.3498(3) 0.1418(2) 0.0228(8) Uani d 1 . .
C C22 -0.2298(3) 0.6735(4) 0.2654(3) 0.0376(11) Uani d 1 . .
H H22A -0.227242 0.648711 0.321884 0.056 Uiso calc 1 . .
H H22B -0.287159 0.670245 0.242760 0.056 Uiso calc 1 . .
H H22C -0.210380 0.743211 0.264595 0.056 Uiso calc 1 . .
O O1 0.3361(2) 0.3945(3) 0.2082(3) 0.0662(12) Uani d 1 . .
C C17 -0.0520(2) 0.7270(3) 0.2483(3) 0.0259(8) Uani d 1 . .
C C18 0.2430(3) 0.2311(4) 0.3431(3) 0.0440(12) Uani d 1 . .
H H18A 0.226643 0.253227 0.397029 0.066 Uiso calc 1 . .
H H18B 0.297676 0.258606 0.332662 0.066 Uiso calc 1 . .
H H18C 0.245274 0.157509 0.341705 0.066 Uiso calc 1 . .
C C19 -0.0596(2) 0.2932(3) 0.2505(3) 0.0303(9) Uani d 1 . .
H H19A -0.066126 0.238515 0.289815 0.045 Uiso calc 1 . .
H H19B -0.092365 0.278275 0.199824 0.045 Uiso calc 1 . .
H H19C -0.078875 0.356300 0.273773 0.045 Uiso calc 1 . .
C C21 0.0581(2) 0.5886(3) 0.1664(3) 0.0304(9) Uani d 1 . .
H H21A 0.091063 0.540315 0.199549 0.046 Uiso calc 1 . .
H H21B 0.067175 0.656430 0.188410 0.046 Uiso calc 1 . .
H H21C 0.074817 0.586262 0.109739 0.046 Uiso calc 1 . .
O O2 0.3294(2) 0.2394(4) 0.1532(2) 0.0708(13) Uani d 1 . .
C C14 0.2970(3) 0.3146(4) 0.1860(3) 0.0372(10) Uani d 1 . .
O O7 -0.03688(19) 0.7326(2) 0.32496(18) 0.0341(7) Uani d 1 . .
N N1 0.5269(4) 0.6220(4) 0.4573(3) 0.0606(13) Uani d 1 . .
O O9 0.5082(4) 0.5566(3) 0.3294(3) 0.0872(16) Uani d 1 . .
C C24 0.5541(6) 0.5858(5) 0.3896(4) 0.087(2) Uani d 1 . .
H H24 0.612314 0.581101 0.385432 0.104 Uiso calc 1 . .
C C25 0.4385(6) 0.6358(7) 0.4696(6) 0.111(3) Uani d 1 . .
H H25A 0.406182 0.618260 0.419280 0.167 Uiso calc 1 . .
H H25B 0.428086 0.706177 0.483597 0.167 Uiso calc 1 . .
H H25C 0.422090 0.592343 0.514326 0.167 Uiso calc 1 . .
C C26 0.5775(7) 0.6482(6) 0.5286(5) 0.118(3) Uani d 1 . .
H H26A 0.628675 0.608593 0.530059 0.177 Uiso calc 1 . .
H H26B 0.547276 0.634093 0.577662 0.177 Uiso calc 1 . .
H H26C 0.591134 0.719925 0.526831 0.177 Uiso calc 1 . .
O O3W 0.3249(2) 0.2465(3) -0.0657(2) 0.0506(9) Uani d 1 . .
H H3WA 0.326639 0.307674 -0.084021 0.061 Uiso d 1 . .
H H3WB 0.281939 0.216674 -0.088641 0.061 Uiso d 1 . .
O O2W 0.5794(2) 0.0158(3) 0.0724(2) 0.0567(10) Uani d 1 . .
O O4W 0.4126(3) -0.0102(3) 0.1332(2) 0.0658(12) Uani d 1 . .
H H4WA 0.420490 -0.070662 0.115231 0.079 Uiso d 1 . .
H H4WB 0.360920 -0.004082 0.144181 0.079 Uiso d 1 . .
O O5W 0.2724(4) 0.0186(7) -0.0006(5) 0.162(3) Uani d 1 . .
H H5WA 0.235027 0.043686 -0.035199 0.194 Uiso d 1 . .
H H5WB 0.243046 0.002587 0.040552 0.194 Uiso d 1 . .
O O6W 0.1923(3) 0.1264(3) -0.1269(2) 0.0676(11) Uani d 1 . .
H H6WA 0.196549 0.102619 -0.175873 0.081 Uiso d 1 . .
H H6WB 0.142909 0.147869 -0.117973 0.081 Uiso d 1 . .
O O7W 0.2391(3) 0.0248(4) 0.1741(3) 0.0860(14) Uani d 1 . .
H H7WA 0.239997 0.084981 0.194632 0.129 Uiso d 1 . .
H H7WB 0.212761 -0.015072 0.205710 0.129 Uiso d 1 . .
H H1WA 0.498(3) 0.386(3) -0.006(3) 0.027(13) Uiso d 1 . .
H H1WB 0.414(5) 0.415(5) 0.003(4) 0.09(2) 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
Ba1 0.01685(13) 0.02292(14) 0.02587(15) -0.00069(9) 0.00089(10) 0.00247(9)
Ba2 0.02899(15) 0.02361(14) 0.02588(15) 0.00047(10) 0.00718(11) 0.00129(9)
O5 0.0212(16) 0.053(2) 0.053(2) 0.0006(14) -0.0127(15) 0.0130(16)
O1W 0.0342(18) 0.0355(18) 0.0254(16) 0.0047(15) 0.0062(15) -0.0007(13)
O8 0.0394(18) 0.0286(16) 0.0385(18) -0.0057(14) 0.0002(14) -0.0026(14)
C15 0.0153(17) 0.029(2) 0.0227(19) -0.0004(15) 0.0020(15) 0.0005(16)
O4 0.0365(16) 0.0219(15) 0.0315(16) -0.0052(12) 0.0072(13) 0.0006(12)
C3 0.0192(17) 0.0229(17) 0.0218(17) 0.0010(14) 0.0053(14) -0.0023(14)
O3 0.0423(17) 0.0297(16) 0.0290(16) -0.0032(13) 0.0143(14) -0.0039(13)
C13 0.0152(16) 0.0262(18) 0.0249(17) 0.0021(14) -0.0006(14) 0.0036(15)
C2 0.0178(17) 0.0303(19) 0.0248(18) 0.0008(15) 0.0035(15) 0.0003(15)
C16 0.0165(18) 0.030(2) 0.038(2) -0.0001(16) -0.0020(17) -0.0010(18)
C9 0.0163(16) 0.0250(17) 0.0228(17) -0.0011(14) -0.0024(14) 0.0024(14)
C8 0.0165(16) 0.0242(17) 0.0222(17) 0.0018(14) 0.0009(14) 0.0004(14)
C4 0.0154(16) 0.0256(17) 0.0240(17) -0.0009(14) 0.0052(14) -0.0018(15)
C5 0.0181(16) 0.0253(17) 0.0242(17) 0.0003(14) 0.0039(15) -0.0007(14)
C1 0.0169(17) 0.0321(19) 0.0272(19) 0.0043(15) 0.0064(15) 0.0017(16)
C12 0.0187(17) 0.0246(18) 0.0276(18) 0.0011(15) -0.0021(15) -0.0018(15)
C7 0.0186(17) 0.0301(19) 0.0233(18) 0.0017(15) 0.0024(15) -0.0020(15)
O6 0.0209(17) 0.082(3) 0.079(3) -0.0121(17) 0.0006(18) 0.042(2)
C11 0.0160(17) 0.0284(19) 0.0272(18) 0.0019(15) 0.0023(15) 0.0024(15)
C20 0.028(2) 0.054(3) 0.037(2) 0.007(2) 0.016(2) 0.011(2)
C23 0.022(2) 0.031(2) 0.040(2) -0.0006(17) -0.0048(18) -0.0059(19)
C10 0.0136(16) 0.0266(18) 0.0285(19) -0.0003(14) 0.0013(15) 0.0034(15)
C6 0.0168(16) 0.0281(18) 0.0237(18) 0.0037(14) 0.0047(15) 0.0014(15)
C22 0.022(2) 0.044(3) 0.047(3) 0.0059(19) 0.005(2) -0.009(2)
O1 0.0238(18) 0.091(3) 0.084(3) -0.017(2) 0.0043(19) 0.027(2)
C17 0.0129(17) 0.031(2) 0.033(2) 0.0033(15) -0.0029(16) -0.0044(18)
C18 0.025(2) 0.072(3) 0.035(2) 0.012(2) 0.0031(19) 0.014(2)
C19 0.0179(19) 0.040(2) 0.033(2) -0.0011(17) 0.0031(17) 0.0095(18)
C21 0.0185(19) 0.030(2) 0.043(2) -0.0011(16) 0.0042(18) -0.0036(19)
O2 0.038(2) 0.128(4) 0.048(2) 0.045(2) 0.0142(17) -0.002(2)
C14 0.020(2) 0.060(3) 0.031(2) 0.005(2) 0.0048(18) 0.013(2)
O7 0.0336(17) 0.0384(17) 0.0295(17) -0.0015(14) -0.0066(13) -0.0053(13)
N1 0.087(4) 0.051(3) 0.044(3) -0.005(3) 0.013(3) -0.004(2)
O9 0.159(5) 0.057(3) 0.043(2) 0.007(3) -0.014(3) -0.0116(19)
C24 0.150(6) 0.055(4) 0.056(4) 0.005(4) 0.013(4) 0.007(3)
C25 0.124(7) 0.088(5) 0.127(6) 0.003(5) 0.048(5) 0.031(5)
C26 0.198(8) 0.080(5) 0.073(5) -0.022(5) -0.029(5) 0.008(4)
O3W 0.044(2) 0.052(2) 0.054(2) -0.0051(17) -0.0148(17) 0.0039(17)
O2W 0.050(2) 0.060(2) 0.060(2) 0.0113(19) -0.0008(19) -0.0136(19)
O4W 0.093(3) 0.037(2) 0.070(3) 0.000(2) 0.036(2) 0.0077(18)
O5W 0.084(4) 0.280(10) 0.124(6) 0.069(5) 0.025(4) 0.084(6)
O6W 0.056(2) 0.087(3) 0.058(2) -0.005(2) -0.012(2) 0.002(2)
O7W 0.077(3) 0.070(3) 0.111(4) 0.000(3) 0.012(3) -0.004(3)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 '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'
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
O5 Ba1 Ba2 1_655 . 107.48(7) ?
O5 Ba1 C16 1_655 1_655 22.08(9) ?
O5 Ba1 C17 1_655 2_545 107.99(9) ?
O1W Ba1 Ba2 . . 40.26(6) ?
O1W Ba1 O5 . 1_655 83.19(10) ?
O1W Ba1 C16 . 1_655 96.55(11) ?
O1W Ba1 C17 . 2_545 93.73(10) ?
O1W Ba1 O7 . 2_545 71.04(9) ?
O8 Ba1 Ba2 2_545 . 76.92(7) ?
O8 Ba1 O5 2_545 1_655 113.16(9) ?
O8 Ba1 O1W 2_545 . 116.01(9) ?
O8 Ba1 C16 2_545 1_655 91.47(10) ?
O8 Ba1 O6 2_545 1_655 69.83(10) ?
O8 Ba1 C17 2_545 2_545 22.75(10) ?
O8 Ba1 O7 2_545 2_545 45.51(9) ?
O4 Ba1 Ba2 2 . 117.34(6) ?
O4 Ba1 O5 2 1_655 72.98(8) ?
O4 Ba1 O1W 2 . 79.94(9) ?
O4 Ba1 O8 2 2_545 162.96(9) ?
O4 Ba1 C16 2 1_655 92.58(10) ?
O4 Ba1 O6 2 1_655 112.31(10) ?
O4 Ba1 C17 2 2_545 173.49(9) ?
O4 Ba1 O7 2 2_545 150.96(8) ?
C16 Ba1 Ba2 1_655 . 107.79(7) ?
O6 Ba1 Ba2 1_655 . 104.65(9) ?
O6 Ba1 O5 1_655 1_655 43.95(9) ?
O6 Ba1 O1W 1_655 . 108.46(12) ?
O6 Ba1 C16 1_655 1_655 21.88(10) ?
O6 Ba1 C17 1_655 2_545 71.02(10) ?
O6 Ba1 O7 1_655 2_545 77.25(10) ?
O1 Ba1 Ba2 . . 70.21(10) ?
O1 Ba1 O5 . 1_655 160.52(10) ?
O1 Ba1 O1W . . 83.57(12) ?
O1 Ba1 O8 . 2_545 85.54(11) ?
O1 Ba1 O4 . 2 90.68(11) ?
O1 Ba1 C16 . 1_655 176.71(12) ?
O1 Ba1 O6 . 1_655 155.30(11) ?
O1 Ba1 C17 . 2_545 87.07(11) ?
O1 Ba1 O7 . 2_545 86.97(12) ?
C17 Ba1 Ba2 2_545 . 56.15(7) ?
C17 Ba1 C16 2_545 1_655 89.64(10) ?
O7 Ba1 Ba2 2_545 . 35.53(6) ?
O7 Ba1 O5 2_545 1_655 102.09(9) ?
O7 Ba1 C16 2_545 1_655 89.96(9) ?
O7 Ba1 C17 2_545 2_545 22.82(9) ?
O9 Ba1 Ba2 . . 150.78(10) ?
O9 Ba1 O5 . 1_655 96.38(14) ?
O9 Ba1 O1W . . 164.67(12) ?
O9 Ba1 O8 . 2_545 78.33(11) ?
O9 Ba1 O4 . 2 85.27(11) ?
O9 Ba1 C16 . 1_655 88.07(15) ?
O9 Ba1 O6 . 1_655 80.86(16) ?
O9 Ba1 O1 . . 92.66(16) ?
O9 Ba1 C17 . 2_545 100.93(12) ?
O9 Ba1 O7 . 2_545 123.74(11) ?
O1W Ba2 Ba1 . . 37.64(6) ?
O1W Ba2 O2W . 3_655 134.36(10) ?
O1W Ba2 O2W . . 124.29(11) ?
O1W Ba2 O5W . . 129.83(14) ?
O3 Ba2 Ba1 4_665 . 93.46(6) ?
O3 Ba2 O1W 4_665 . 68.29(9) ?
O3 Ba2 O2W 4_665 . 73.90(10) ?
O3 Ba2 O2W 4_665 3_655 76.28(10) ?
O3 Ba2 O5W 4_665 . 120.04(14) ?
O2 Ba2 Ba1 . . 59.45(11) ?
O2 Ba2 O1W . . 78.70(13) ?
O2 Ba2 O3 . 4_665 146.90(12) ?
O2 Ba2 O2W . . 130.43(11) ?
O2 Ba2 O2W . 3_655 129.85(13) ?
O2 Ba2 O4W . . 81.44(13) ?
O2 Ba2 O5W . . 79.55(16) ?
O7 Ba2 Ba1 2_545 . 39.33(6) ?
O7 Ba2 O1W 2_545 . 72.11(9) ?
O7 Ba2 O3 2_545 4_665 96.02(10) ?
O7 Ba2 O2 2_545 . 75.32(11) ?
O7 Ba2 O3W 2_545 . 135.95(10) ?
O7 Ba2 O2W 2_545 3_655 141.17(10) ?
O7 Ba2 O2W 2_545 . 72.91(10) ?
O7 Ba2 O4W 2_545 . 88.65(11) ?
O7 Ba2 O5W 2_545 . 142.01(13) ?
O3W Ba2 Ba1 . . 96.61(8) ?
O3W Ba2 O1W . . 67.05(10) ?
O3W Ba2 O3 . 4_665 83.93(10) ?
O3W Ba2 O2 . . 81.13(11) ?
O3W Ba2 O2W . 3_655 81.79(11) ?
O3W Ba2 O2W . . 146.09(11) ?
O3W Ba2 O4W . . 124.12(13) ?
O3W Ba2 O5W . . 65.26(14) ?
O2W Ba2 Ba1 . . 109.82(7) ?
O2W Ba2 Ba1 3_655 . 169.71(8) ?
O2W Ba2 O2W . 3_655 68.37(12) ?
O2W Ba2 O5W . . 104.12(15) ?
O2W Ba2 O5W 3_655 . 50.52(15) ?
O4W Ba2 Ba1 . . 118.26(9) ?
O4W Ba2 O1W . . 155.21(10) ?
O4W Ba2 O3 . 4_665 130.91(11) ?
O4W Ba2 O2W . 3_655 70.30(12) ?
O4W Ba2 O2W . . 60.93(12) ?
O4W Ba2 O5W . . 59.51(15) ?
O5W Ba2 Ba1 . . 137.76(13) ?
C16 O5 Ba1 . 1_455 90.4(3) ?
Ba1 O1W Ba2 . . 102.09(10) ?
Ba1 O1W H1WA . . 118(3) ?
Ba1 O1W H1WB . . 110(4) ?
Ba2 O1W H1WA . . 100(3) ?
Ba2 O1W H1WB . . 111(4) ?
H1WA O1W H1WB . . 114(5) ?
C17 O8 Ba1 . 2 98.8(2) ?
O4 C15 C3 . . 120.1(3) ?
O4 C15 O3 . . 124.4(4) ?
O3 C15 C3 . . 115.6(3) ?
C15 O4 Ba1 . 2_545 144.8(3) ?
C2 C3 C15 . . 119.2(3) ?
C2 C3 C4 . . 121.9(3) ?
C4 C3 C15 . . 118.8(3) ?
C15 O3 Ba2 . 4_566 139.5(3) ?
C8 C13 C12 . . 119.8(3) ?
C8 C13 C21 . . 121.7(3) ?
C12 C13 C21 . . 118.5(4) ?
C3 C2 C1 . . 118.1(4) ?
C3 C2 C18 . . 120.4(4) ?
C1 C2 C18 . . 121.5(3) ?
O5 C16 Ba1 . 1_455 67.5(2) ?
O5 C16 O6 . . 122.5(4) ?
O5 C16 C10 . . 120.3(4) ?
O6 C16 Ba1 . 1_455 55.0(2) ?
O6 C16 C10 . . 117.2(4) ?
C10 C16 Ba1 . 1_455 171.9(3) ?
C8 C9 C23 . . 122.2(4) ?
C10 C9 C8 . . 118.9(3) ?
C10 C9 C23 . . 119.0(3) ?
C13 C8 C9 . . 119.4(3) ?
C13 C8 C7 . . 119.2(3) ?
C9 C8 C7 . . 121.3(3) ?
C3 C4 C5 . . 120.0(3) ?
C3 C4 C19 . . 118.2(3) ?
C5 C4 C19 . . 121.8(3) ?
C4 C5 C7 . . 120.5(3) ?
C4 C5 C6 . . 118.7(3) ?
C6 C5 C7 . . 120.8(3) ?
C2 C1 C6 . . 121.9(3) ?
C2 C1 C14 . . 119.0(4) ?
C6 C1 C14 . . 119.1(3) ?
C13 C12 C17 . . 119.6(3) ?
C11 C12 C13 . . 120.9(4) ?
C11 C12 C17 . . 119.4(3) ?
C8 C7 C5 . . 115.9(3) ?
C8 C7 H7A . . 108.3 ?
C8 C7 H7B . . 108.3 ?
C5 C7 H7A . . 108.3 ?
C5 C7 H7B . . 108.3 ?
H7A C7 H7B . . 107.4 ?
C16 O6 Ba1 . 1_455 103.1(3) ?
C12 C11 C22 . . 120.7(4) ?
C10 C11 C12 . . 117.8(4) ?
C10 C11 C22 . . 121.5(3) ?
H20A C20 H20B . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
C6 C20 H20A . . 109.5 ?
C6 C20 H20B . . 109.5 ?
C6 C20 H20C . . 109.5 ?
C9 C23 H23A . . 109.5 ?
C9 C23 H23B . . 109.5 ?
C9 C23 H23C . . 109.5 ?
H23A C23 H23B . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C9 C10 C16 . . 118.9(3) ?
C11 C10 C16 . . 118.7(3) ?
C11 C10 C9 . . 122.3(3) ?
C5 C6 C20 . . 122.4(4) ?
C1 C6 C5 . . 119.3(3) ?
C1 C6 C20 . . 118.2(3) ?
C11 C22 H22A . . 109.5 ?
C11 C22 H22B . . 109.5 ?
C11 C22 H22C . . 109.5 ?
H22A C22 H22B . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C14 O1 Ba1 . . 130.3(3) ?
O8 C17 Ba1 . 2 58.4(2) ?
O8 C17 C12 . . 116.1(4) ?
C12 C17 Ba1 . 2 171.7(3) ?
O7 C17 Ba1 . 2 65.8(2) ?
O7 C17 O8 . . 124.0(4) ?
O7 C17 C12 . . 119.9(4) ?
C2 C18 H18A . . 109.5 ?
C2 C18 H18B . . 109.5 ?
C2 C18 H18C . . 109.5 ?
H18A C18 H18B . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C4 C19 H19A . . 109.5 ?
C4 C19 H19B . . 109.5 ?
C4 C19 H19C . . 109.5 ?
H19A C19 H19B . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C13 C21 H21A . . 109.5 ?
C13 C21 H21B . . 109.5 ?
C13 C21 H21C . . 109.5 ?
H21A C21 H21B . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C14 O2 Ba2 . . 148.9(4) ?
O1 C14 C1 . . 117.1(4) ?
O2 C14 C1 . . 118.2(5) ?
O2 C14 O1 . . 124.8(5) ?
Ba2 O7 Ba1 2 2 105.14(9) ?
C17 O7 Ba1 . 2 91.4(2) ?
C17 O7 Ba2 . 2 145.2(3) ?
C24 N1 C25 . . 122.6(7) ?
C24 N1 C26 . . 125.3(8) ?
C26 N1 C25 . . 112.0(7) ?
C24 O9 Ba1 . . 146.6(6) ?
N1 C24 H24 . . 117.8 ?
O9 C24 N1 . . 124.5(9) ?
O9 C24 H24 . . 117.8 ?
N1 C25 H25A . . 109.5 ?
N1 C25 H25B . . 109.5 ?
N1 C25 H25C . . 109.5 ?
H25A C25 H25B . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
N1 C26 H26A . . 109.5 ?
N1 C26 H26B . . 109.5 ?
N1 C26 H26C . . 109.5 ?
H26A C26 H26B . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
Ba2 O3W H3WA . . 124.8 ?
Ba2 O3W H3WB . . 126.5 ?
H3WA O3W H3WB . . 108.6 ?
Ba2 O2W Ba2 . 3_655 111.63(12) ?
Ba2 O4W H4WA . . 124.7 ?
Ba2 O4W H4WB . . 101.9 ?
H4WA O4W H4WB . . 108.5 ?
Ba2 O5W H5WA . . 116.4 ?
Ba2 O5W H5WB . . 115.4 ?
H5WA O5W H5WB . . 102.0 ?
H6WA O6W H6WB . . 113.2 ?
H7WA O7W H7WB . . 109.4 ?
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
Ba1 Ba2 . 4.4483(9) ?
Ba1 O5 1_655 3.035(3) ?
Ba1 O1W . 2.778(3) ?
Ba1 O8 2_545 2.760(3) ?
Ba1 O4 2 2.745(3) ?
Ba1 C16 1_655 3.286(4) ?
Ba1 O6 1_655 2.764(3) ?
Ba1 O1 . 2.705(3) ?
Ba1 C17 2_545 3.201(4) ?
Ba1 O7 2_545 2.921(3) ?
Ba1 O9 . 2.665(4) ?
Ba2 O1W . 2.940(3) ?
Ba2 O3 4_665 2.721(3) ?
Ba2 O2 . 2.699(3) ?
Ba2 O7 2_545 2.678(3) ?
Ba2 O3W . 2.694(3) ?
Ba2 O2W . 2.955(4) ?
Ba2 O2W 3_655 3.013(4) ?
Ba2 O4W . 2.713(3) ?
Ba2 O5W . 3.297(9) ?
O5 C16 . 1.235(5) ?
O1W H1WA . 0.77(5) ?
O1W H1WB . 0.89(8) ?
O8 C17 . 1.252(5) ?
C15 O4 . 1.245(5) ?
C15 C3 . 1.517(5) ?
C15 O3 . 1.259(5) ?
C3 C2 . 1.389(5) ?
C3 C4 . 1.394(5) ?
C13 C8 . 1.400(5) ?
C13 C12 . 1.406(5) ?
C13 C21 . 1.503(5) ?
C2 C1 . 1.394(6) ?
C2 C18 . 1.508(6) ?
C16 O6 . 1.257(5) ?
C16 C10 . 1.522(5) ?
C9 C8 . 1.404(5) ?
C9 C23 . 1.512(5) ?
C9 C10 . 1.398(5) ?
C8 C7 . 1.525(5) ?
C4 C5 . 1.407(5) ?
C4 C19 . 1.510(5) ?
C5 C7 . 1.529(5) ?
C5 C6 . 1.419(5) ?
C1 C6 . 1.400(6) ?
C1 C14 . 1.508(6) ?
C12 C11 . 1.400(5) ?
C12 C17 . 1.517(6) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C11 C10 . 1.390(6) ?
C11 C22 . 1.511(6) ?
C20 H20A . 0.9600 ?
C20 H20B . 0.9600 ?
C20 H20C . 0.9600 ?
C20 C6 . 1.510(5) ?
C23 H23A . 0.9600 ?
C23 H23B . 0.9600 ?
C23 H23C . 0.9600 ?
C22 H22A . 0.9600 ?
C22 H22B . 0.9600 ?
C22 H22C . 0.9600 ?
O1 C14 . 1.253(6) ?
C17 O7 . 1.242(5) ?
C18 H18A . 0.9600 ?
C18 H18B . 0.9600 ?
C18 H18C . 0.9600 ?
C19 H19A . 0.9600 ?
C19 H19B . 0.9600 ?
C19 H19C . 0.9600 ?
C21 H21A . 0.9600 ?
C21 H21B . 0.9600 ?
C21 H21C . 0.9600 ?
O2 C14 . 1.237(6) ?
N1 C24 . 1.278(8) ?
N1 C25 . 1.434(10) ?
N1 C26 . 1.402(9) ?
O9 C24 . 1.236(9) ?
C24 H24 . 0.9300 ?
C25 H25A . 0.9600 ?
C25 H25B . 0.9600 ?
C25 H25C . 0.9600 ?
C26 H26A . 0.9600 ?
C26 H26B . 0.9600 ?
C26 H26C . 0.9600 ?
O3W H3WA . 0.8500 ?
O3W H3WB . 0.8499 ?
O4W H4WA . 0.8500 ?
O4W H4WB . 0.8500 ?
O5W H5WA . 0.8537 ?
O5W H5WB . 0.8537 ?
O6W H6WA . 0.8499 ?
O6W H6WB . 0.8499 ?
O7W H7WA . 0.8502 ?
O7W H7WB . 0.8501 ?
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
C26 H26B O8 4_676 0.96 2.60 3.458(11) 149.1 no
O3W H3WA O5 3_565 0.85 1.96 2.798(5) 169.0 no
O3W H3WB O6W . 0.85 1.92 2.756(5) 168.5 no
O4W H4WA O3 2_545 0.85 1.95 2.797(5) 174.8 no
O4W H4WB O7W . 0.85 2.05 2.894(7) 174.5 no
O5W H5WA O6W . 0.85 1.92 2.720(7) 156.4 no
O5W H5WB O7W . 0.85 2.16 2.879(9) 141.1 no
O6W H6WA O6 4_665 0.85 1.84 2.660(5) 163.0 no
O6W H6WB O8 3_565 0.85 2.13 2.774(5) 132.8 no
O1W H1WA O4 4_665 0.77(5) 2.03(5) 2.754(4) 158(5) no
O1W H1WB O5 3_565 0.89(8) 2.11(7) 2.856(4) 141(6) no
_cod_database_fobs_code 2022382