#------------------------------------------------------------------------------
#$Date: 2022-05-25 02:56:34 +0100 (Wed, 25 May 2022) $
#$Revision: 275637 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244104.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_2244104
loop_
_publ_author_name
'Ruzmetov, Abror'
'Ibragimov, Aziz'
'Ashurov, Jamshid'
'Boltaeva, Zebo'
'Ibragimov, Bakhtiyar'
'Usmanov, Sultan'
_publ_section_title
;
Synthesis, crystal structure and Hirshfeld surface analysis of
hexaaquanickel(II) bis(4-hydroxybenzoate) dihydrate
;
_journal_coeditor_code YZ2020
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S205698902200531X
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac '[Ni (H2 O)6] (C7 H5 O3)2, 2H2 O'
_chemical_formula_moiety 'H12 Ni O6 2+, 2(C7 H5 O3 -), 2(H2 O)'
_chemical_formula_sum 'C14 H26 Ni O14'
_chemical_formula_weight 477.06
_chemical_name_systematic
;
Hexaaquanickel(II) bis(4-hydroxybenzoate) dihydrate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_atom_sites_solution_hydrogens mixed
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.0812(2)
_cell_length_b 7.63258(17)
_cell_length_c 23.7986(5)
_cell_measurement_reflns_used 4076
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 70.4770
_cell_measurement_theta_min 3.7160
_cell_volume 2012.84(7)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018/2 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, single source at home/near, HyPix3000'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0332
_diffrn_reflns_av_unetI/netI 0.0267
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 9865
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 71.577
_diffrn_reflns_theta_min 3.715
_exptl_absorpt_coefficient_mu 2.045
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.36167
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour 'clear greenish green'
_exptl_crystal_density_diffrn 1.574
_exptl_crystal_description prism
_exptl_crystal_F_000 1000
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.247
_refine_diff_density_min -0.432
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 169
_refine_ls_number_reflns 1949
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.050
_refine_ls_R_factor_all 0.0400
_refine_ls_R_factor_gt 0.0338
_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^)+(0.0601P)^2^+0.4799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0964
_refine_ls_wR_factor_ref 0.1012
_reflns_number_gt 1656
_reflns_number_total 1949
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2020sup1.cif
_cod_data_source_block I
_cod_database_code 2244104
_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 0.685
_shelx_estimated_absorpt_t_max 0.749
_shelx_hkl_file
;
-1 0 0 -0.02 0.11
-1 0 0 -0.02 0.10
1 0 0 0.13 0.07
-1 0 0 0.26 0.25
-1 0 0 -0.28 0.18
-2 0 0 850.56 32.52
-2 0 0 843.94 32.52
2 0 0 805.97 32.27
2 0 0 847.24 32.26
-2 0 0 853.17 32.98
-2 0 0 834.42 32.67
-3 0 0 -0.07 0.45
-3 0 0 0.08 0.38
-3 0 0 0.71 0.41
3 0 0 0.04 0.22
-3 0 0 -0.12 0.83
-3 0 0 -0.45 0.68
-4 0 0 2657.35 101.37
-4 0 0 2577.63 101.38
-4 0 0 2618.04 101.72
-5 0 0 -0.30 0.59
-5 0 0 0.49 0.78
-6 0 0 927.89 37.88
-6 0 0 945.76 37.92
-7 0 0 -0.46 0.94
-8 0 0 254.87 11.65
-8 0 0 278.28 12.01
-8 0 0 240.70 11.52
-9 0 0 -0.43 0.96
-9 0 0 0.82 0.87
-10 0 0 63.22 4.35
-10 0 0 65.51 4.31
-10 0 0 62.01 4.28
-11 0 0 -1.09 1.16
-11 0 0 -0.40 0.92
-11 0 0 1.27 0.98
-11 0 0 0.44 0.91
-12 0 0 99.92 5.65
-12 0 0 107.75 5.61
-13 0 0 -0.37 0.53
0 1 0 -0.04 0.19
0 1 0 0.45 0.20
0 1 0 0.24 0.14
0 1 0 0.08 0.18
0 1 0 0.43 0.16
0 1 0 -0.05 0.21
-1 -1 0 0.55 0.16
-1 -1 0 0.84 0.21
-1 1 0 0.99 0.20
1 1 0 0.49 0.22
-1 1 0 0.58 0.18
1 1 0 0.95 0.31
-1 1 0 0.15 0.10
1 1 0 0.46 0.23
-2 1 0 818.08 30.82
-2 -1 0 731.11 30.74
-2 1 0 816.54 30.82
-2 -1 0 774.11 30.79
2 1 0 806.53 31.00
2 1 0 812.35 30.91
-2 -1 0 791.73 30.70
-3 -1 0 0.53 0.28
-3 1 0 0.55 0.28
-3 1 0 0.41 0.27
-3 -1 0 0.31 0.32
-3 1 0 0.79 0.39
3 1 0 -0.08 0.39
3 1 0 0.23 0.27
-4 1 0 671.45 24.87
-4 -1 0 606.26 24.72
-4 1 0 639.52 24.82
-4 -1 0 627.03 24.80
4 1 0 580.72 24.56
-4 -1 0 562.85 26.13
-4 -1 0 609.74 25.64
-5 -1 0 0.73 0.44
-5 1 0 0.15 0.47
-5 -1 0 2.15 1.43
-5 -1 0 -0.20 1.02
-6 1 0 20.30 2.05
-6 -1 0 18.69 1.99
-6 -1 0 16.66 2.51
-6 -1 0 19.61 2.24
-7 -1 0 1.12 1.31
-8 -1 0 -0.18 1.16
-8 -1 0 1.50 1.24
-8 1 0 0.90 1.03
-8 1 0 2.31 1.04
-9 -1 0 -2.28 1.85
-9 1 0 -0.62 1.28
-9 -1 0 -1.66 1.28
-9 1 0 0.19 0.91
-9 1 0 -0.22 1.09
-10 -1 0 383.33 17.31
-10 1 0 410.61 17.45
-10 1 0 401.24 17.23
-10 -1 0 386.61 17.26
-10 1 0 418.87 17.62
-10 1 0 371.46 17.25
-11 1 0 2.29 0.90
-11 1 0 -0.57 1.13
-11 -1 0 -0.81 1.07
-11 1 0 0.22 0.96
-11 1 0 0.21 0.73
-12 1 0 99.82 5.35
-12 -1 0 109.33 5.60
-12 -1 0 96.51 5.54
-13 -1 0 0.12 0.53
-13 -1 0 0.35 0.65
0 2 0 9966.53 382.13
0 2 0 9999.00 382.25
0 2 0 9920.03 382.21
0 2 0 9963.30 381.87
-1 2 0 -0.22 0.40
1 2 0 0.43 0.44
1 2 0 0.28 0.58
1 2 0 0.24 0.72
-1 2 0 0.52 0.23
1 2 0 0.79 0.38
1 2 0 0.50 0.43
2 2 0 3281.22 128.05
-2 2 0 3250.06 127.63
2 2 0 3372.47 127.83
2 2 0 3375.20 128.10
-3 2 0 0.08 0.29
3 2 0 0.68 0.32
3 2 0 0.80 0.54
-4 2 0 132.78 6.15
4 2 0 138.16 6.42
4 2 0 123.05 6.46
5 2 0 -0.16 0.55
-5 -2 0 -0.32 1.53
-6 -2 0 613.43 28.41
-6 -2 0 653.84 27.56
-7 -2 0 0.35 0.57
-7 2 0 0.66 0.81
-8 2 0 218.85 10.14
-8 -2 0 203.46 11.43
-9 2 0 0.22 1.11
-9 -2 0 -0.35 1.31
-10 2 0 2.93 1.27
-10 -2 0 3.14 1.24
-10 2 0 2.06 1.02
-11 2 0 -0.75 0.92
-11 -2 0 0.19 0.91
-11 2 0 1.04 0.87
-12 -2 0 5.29 1.15
-12 -2 0 5.51 1.11
-13 -2 0 0.10 0.51
-13 -2 0 0.22 0.51
0 3 0 0.52 0.36
0 3 0 0.13 0.54
-1 3 0 0.46 0.47
1 3 0 0.48 0.77
1 3 0 1.05 0.52
2 3 0 817.11 32.74
-2 3 0 785.27 32.37
2 3 0 819.77 32.52
2 3 0 848.35 33.33
3 3 0 3.48 0.79
-3 3 0 0.12 0.44
4 3 0 27.74 2.35
5 3 0 2.99 0.84
6 3 0 239.18 11.58
-7 -3 0 0.52 2.16
-7 -3 0 0.64 0.84
-8 -3 0 0.92 1.79
-8 -3 0 -0.23 0.75
-9 3 0 0.20 1.09
-9 -3 0 0.24 0.87
9 3 0 0.30 1.07
-10 3 0 276.41 12.37
-10 -3 0 252.43 12.34
10 3 0 284.29 13.30
11 3 0 -0.26 0.92
-12 -3 0 81.20 4.41
0 4 0 497.05 20.88
1 4 0 0.72 0.47
1 4 0 0.21 0.83
2 4 0 4650.74 183.66
2 4 0 4899.95 184.48
3 4 0 0.59 0.66
-3 4 0 -0.17 0.52
3 4 0 0.84 1.28
4 4 0 642.47 28.87
4 4 0 688.99 28.06
5 4 0 1.76 1.01
-5 4 0 -0.40 0.99
5 4 0 0.79 0.97
-5 4 0 0.43 0.58
-6 4 0 339.19 14.83
6 4 0 339.12 15.51
-6 4 0 320.94 14.07
6 4 0 309.80 14.92
-7 -4 0 -0.66 2.53
7 4 0 -1.32 1.57
-7 -4 0 -0.24 0.75
7 4 0 0.82 1.12
-7 4 0 0.34 0.72
-8 -4 0 0.25 0.90
8 4 0 1.14 1.20
9 4 0 0.56 0.98
-9 -4 0 -0.24 0.81
-10 -4 0 1.67 0.88
10 4 0 1.28 1.26
11 4 0 0.62 0.85
12 4 0 1.24 0.67
0 5 0 0.57 0.60
1 5 0 -0.26 0.86
-1 5 0 -0.37 1.02
1 5 0 -0.14 0.61
-1 5 0 0.29 0.59
2 5 0 302.97 14.47
2 5 0 317.29 14.02
-2 5 0 302.65 13.18
-2 5 0 304.50 13.69
-3 5 0 0.71 0.69
3 5 0 1.51 0.98
-3 5 0 -0.15 0.74
-3 5 0 -0.20 0.99
-4 5 0 226.20 11.00
-4 5 0 231.49 10.43
4 5 0 230.83 11.52
-4 5 0 238.26 10.99
-5 5 0 -0.17 0.73
5 5 0 0.61 1.58
-5 5 0 -0.48 0.99
-6 5 0 -0.54 0.79
6 5 0 0.54 1.14
6 5 0 -0.99 1.72
-6 5 0 1.28 0.95
7 5 0 -0.83 1.06
-7 -5 0 -0.24 0.80
-7 5 0 -0.36 0.89
8 5 0 178.13 9.40
-8 -5 0 181.85 9.10
-8 5 0 177.19 8.53
-9 -5 0 -0.63 0.82
9 5 0 0.48 1.06
10 5 0 17.94 2.04
-10 -5 0 17.85 1.84
11 5 0 -0.43 0.66
0 6 0 60.06 3.78
0 6 0 51.93 4.09
-1 6 0 0.91 0.87
1 6 0 -0.18 0.82
-2 6 0 130.01 6.85
-2 6 0 143.29 7.50
-3 6 0 1.01 0.82
-3 6 0 1.43 0.85
-3 6 0 -0.96 1.50
-4 6 0 646.09 26.65
-4 6 0 649.08 27.27
-5 6 0 0.74 0.93
-6 6 0 15.86 1.86
-6 -6 0 11.36 1.69
-6 -6 0 15.84 3.49
-7 6 0 -0.18 0.94
-7 -6 0 -0.21 0.64
-8 6 0 -0.16 0.74
8 6 0 -0.42 0.82
-8 -6 0 -0.18 0.64
-9 -6 0 0.15 0.47
9 6 0 0.17 0.71
10 6 0 29.98 2.18
0 7 0 0.40 0.75
0 7 0 1.44 1.10
1 7 0 -1.17 0.90
-1 7 0 1.41 1.07
-1 7 0 0.50 1.51
-2 7 0 -0.20 0.81
-2 7 0 -1.01 1.58
-3 7 0 1.70 0.89
-3 7 0 5.50 1.71
-4 7 0 9.58 1.47
-4 7 0 14.55 2.22
-5 7 0 1.37 0.96
-5 -7 0 0.44 2.25
-5 7 0 -1.08 1.18
-6 7 0 9.86 1.51
-6 -7 0 9.03 2.58
-7 7 0 0.85 0.87
-8 -7 0 -0.12 0.39
0 8 0 36.81 2.86
0 8 0 41.06 3.21
-1 8 0 0.18 0.77
1 8 0 -0.33 0.80
-1 8 0 0.84 1.12
-2 8 0 105.39 5.69
-2 8 0 111.71 6.19
-3 8 0 -0.15 0.62
-3 8 0 2.02 1.23
-4 -8 0 115.92 7.54
-5 -8 0 2.15 1.67
-5 8 0 -0.12 0.63
-6 8 0 1.93 0.68
0 9 0 0.33 0.52
1 9 0 -0.20 0.48
-1 9 0 -0.44 0.56
-2 -9 0 2.48 1.67
-3 -9 0 -0.81 1.26
-1 0 -1 0.03 0.13
1 0 1 0.66 0.12
1 0 -1 0.10 0.07
-1 0 -1 0.04 0.20
-1 0 -1 0.15 0.24
-1 0 1 -0.02 0.11
-1 0 1 -0.04 0.19
-1 0 1 0.06 0.31
-2 0 -1 0.22 0.27
-2 0 -1 -0.16 0.22
2 0 1 -0.03 0.16
-2 0 1 0.21 0.25
2 0 -1 0.32 0.16
-2 0 1 -0.19 0.57
-2 0 1 0.21 0.31
-2 0 -1 0.24 0.53
-2 0 -1 -0.08 0.46
-3 0 1 -0.24 0.34
-3 0 -1 0.16 0.41
-3 0 -1 -0.32 0.33
3 0 -1 -0.21 0.23
3 0 1 0.28 0.27
-3 0 -1 -0.10 0.64
-3 0 -1 -0.44 0.77
-3 0 1 -0.24 0.86
-4 0 -1 0.90 0.44
-4 0 1 0.78 0.38
-4 0 -1 1.22 0.50
-4 0 1 -0.29 0.78
-4 0 -1 -0.13 0.67
-4 0 -1 0.27 0.78
-5 0 1 1.64 0.66
-5 0 -1 0.74 0.52
-5 0 -1 0.59 0.57
-5 0 -1 1.28 0.82
-5 0 1 0.17 0.81
-6 0 1 0.77 0.39
-6 0 1 -0.19 0.84
-6 0 -1 -0.38 0.77
-7 0 1 1.20 0.75
-7 0 1 0.23 0.90
-7 0 -1 -0.68 0.98
-8 0 1 0.37 0.95
-8 0 -1 1.29 0.80
-8 0 1 -0.18 0.83
-8 0 -1 0.20 0.86
-8 0 -1 -1.42 0.90
-9 0 -1 0.21 0.79
-9 0 1 0.21 0.85
-9 0 -1 0.20 0.91
-9 0 -1 -0.41 0.80
-9 0 1 -0.21 0.96
-10 0 -1 2.29 1.07
-10 0 1 0.68 0.91
-10 0 1 0.21 0.92
-10 0 -1 0.63 1.00
-10 0 1 0.22 1.01
-10 0 -1 -0.66 1.06
-11 0 1 0.22 0.82
-11 0 -1 -0.21 0.90
-11 0 -1 -0.20 0.85
-11 0 1 0.22 1.09
-11 0 -1 -0.44 1.13
-11 0 1 0.60 0.93
-12 0 1 -0.18 0.72
-12 0 -1 -0.54 0.71
-12 0 1 1.80 0.77
-12 0 -1 0.84 1.05
-12 0 1 -0.99 1.08
-13 0 1 0.12 0.52
-13 0 -1 0.12 0.46
0 1 1 0.04 0.15
0 1 1 -0.03 0.13
0 1 1 0.29 0.32
0 1 1 0.05 0.26
0 1 -1 -0.10 0.25
0 1 -1 0.08 0.21
0 1 -1 0.75 0.19
0 1 -1 0.31 0.21
-1 1 -1 728.38 27.76
1 1 1 718.64 27.91
-1 1 1 716.43 27.63
-1 -1 -1 690.46 27.72
-1 1 -1 750.00 27.83
1 1 -1 700.33 27.79
1 1 -1 726.18 28.00
1 1 -1 717.56 27.89
-1 1 -1 715.02 27.72
-2 1 -1 2761.40 103.69
-2 -1 -1 2656.11 103.67
-2 -1 -1 2585.11 103.63
2 1 1 2776.66 103.78
-2 1 1 2616.20 103.60
-2 1 -1 2831.34 103.72
2 1 -1 2773.86 103.85
-2 -1 1 2683.95 103.65
2 1 -1 2711.66 103.74
-2 1 1 2738.61 103.67
-2 -1 1 2465.14 104.09
-3 -1 -1 392.84 16.29
-3 1 1 398.08 16.13
-3 1 -1 424.98 16.38
-3 -1 -1 403.09 16.34
3 1 -1 414.71 16.42
-3 1 -1 414.06 16.39
-3 1 1 408.33 16.34
-3 -1 1 393.45 16.31
3 1 -1 392.28 16.28
3 1 1 398.05 16.33
-3 -1 1 416.74 16.28
-4 1 -1 13.37 1.24
-4 1 -1 12.92 1.25
-4 -1 -1 12.24 1.21
-4 -1 -1 15.18 1.30
4 1 -1 8.66 1.01
-4 -1 1 12.47 1.21
4 1 1 17.08 1.32
-4 1 1 12.53 1.21
-4 -1 1 11.53 2.18
-4 -1 -1 7.82 1.68
-4 -1 -1 7.51 1.94
-4 -1 1 11.25 1.61
-5 1 -1 425.81 17.24
-5 -1 -1 396.08 17.09
-5 -1 1 408.40 17.17
-5 1 1 421.27 17.21
-5 -1 -1 391.35 18.21
-5 -1 1 397.69 18.37
-5 -1 1 414.05 17.54
-5 -1 -1 403.40 17.84
-6 -1 1 7.63 1.33
-6 1 1 8.36 1.31
-6 -1 -1 11.26 1.80
-6 -1 1 5.00 1.65
-6 -1 -1 8.40 1.74
-7 -1 -1 384.28 17.07
-7 -1 1 373.45 17.09
-7 1 -1 374.12 15.89
-7 1 1 362.08 16.59
-7 -1 1 366.45 16.60
-8 1 -1 37.67 2.84
-8 -1 -1 31.29 3.33
-8 1 1 35.80 2.80
-8 -1 1 34.41 3.52
-8 -1 1 33.30 2.76
-8 -1 -1 33.79 2.78
-8 1 -1 33.70 2.69
-8 1 -1 33.48 2.81
-8 1 1 32.55 2.76
-8 -1 -1 37.44 2.95
-8 1 -1 34.81 2.85
-9 -1 1 62.61 4.28
-9 -1 -1 65.63 4.35
-9 -1 1 57.01 4.92
-9 1 -1 70.35 4.45
-9 1 1 64.81 4.33
-9 1 1 69.09 4.28
-9 1 -1 66.03 4.26
-9 1 -1 73.11 4.62
-9 1 1 73.36 4.61
-10 1 1 339.67 15.11
-10 -1 -1 340.95 15.14
-10 1 -1 325.43 15.04
-10 -1 1 335.68 15.09
-10 1 1 333.83 14.91
-10 1 -1 348.00 15.02
-10 -1 -1 334.67 15.05
-10 1 1 326.47 15.08
-10 1 1 337.86 15.23
-10 1 -1 342.59 15.28
-11 -1 -1 228.09 10.75
-11 -1 1 220.48 10.69
-11 1 1 226.90 10.76
-11 1 -1 246.20 10.90
-11 1 -1 236.93 10.71
-11 -1 1 236.61 10.80
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1 3 8 14.10 1.99
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3 3 -8 6.67 1.86
3 3 -8 5.30 1.32
3 3 8 7.30 1.25
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3 1 26 2.19 0.92
-3 -1 26 1.72 0.71
-3 1 26 1.99 0.78
-3 -1 -26 3.81 0.96
-3 1 -26 3.99 0.96
-4 1 -26 5.72 1.00
4 -1 26 5.36 1.17
4 1 26 7.37 1.32
-4 -1 26 4.07 0.91
-4 1 26 6.64 1.04
-4 -1 -26 5.47 1.04
-4 1 -26 7.78 1.16
-5 1 -26 0.64 0.52
5 -1 26 0.87 0.64
5 1 26 1.35 0.70
-5 -1 26 0.78 0.47
-5 1 26 1.42 0.55
-5 -1 -26 1.16 0.61
-5 1 -26 0.35 0.52
0 2 -26 104.41 5.61
1 2 -26 3.05 0.91
2 2 -26 134.92 6.63
-2 2 -26 127.41 6.63
3 2 -26 6.06 1.09
-3 2 -26 4.53 0.94
4 2 -26 71.73 4.02
-4 2 -26 74.74 4.00
5 2 -26 21.37 1.68
-5 2 -26 22.75 1.68
0 3 -26 -0.28 0.59
0 3 -26 0.16 0.54
1 3 -26 11.28 1.40
1 3 -26 11.08 1.34
-1 3 -26 11.22 1.39
2 3 -26 8.34 1.18
-2 3 -26 7.70 1.17
-3 3 -26 4.19 0.83
3 3 -26 2.95 0.77
-3 3 -26 5.25 0.89
-4 3 -26 0.41 0.41
-4 3 -26 -0.09 0.44
4 3 -26 0.95 0.50
0 4 -26 20.65 1.70
0 4 26 22.16 1.54
-1 4 -26 -0.23 0.44
1 4 -26 0.67 0.45
-1 4 -26 -0.34 0.42
-1 4 26 0.07 0.26
1 4 26 0.16 0.29
-2 4 -26 22.81 1.80
-2 4 -26 29.56 1.95
0 0 27 -0.36 0.69
-1 0 -27 0.33 0.67
1 0 27 -0.37 0.67
-1 0 27 -0.17 0.60
-2 0 -27 -0.47 0.84
-2 0 27 -1.25 0.87
-3 0 -27 -0.14 0.55
3 0 27 -0.67 0.62
-3 0 27 -0.41 0.58
-4 0 -27 -0.37 0.71
4 0 27 -0.59 0.75
-4 0 27 -0.59 0.77
-5 0 -27 -0.10 0.44
5 0 27 0.12 0.44
-5 0 27 -0.09 0.34
0 -1 27 -0.16 0.75
0 1 27 -0.82 0.85
-1 -1 -27 21.30 1.98
-1 1 -27 25.58 2.12
1 -1 27 18.53 1.97
1 1 27 20.43 2.03
-1 -1 27 21.84 2.02
-1 1 27 22.23 2.02
-2 1 -27 2.91 0.76
-2 -1 -27 3.16 0.85
-2 1 -27 3.03 0.88
2 -1 27 2.76 0.89
2 1 27 2.16 0.85
-2 -1 27 4.27 0.92
-2 1 27 2.38 0.69
-3 -1 -27 32.89 2.40
-3 1 -27 38.00 2.52
3 -1 27 34.54 2.57
3 1 27 30.60 2.50
-3 -1 27 36.00 2.42
-3 1 27 34.42 2.37
-4 1 -27 -0.41 0.49
-4 -1 -27 -0.55 0.52
-4 1 -27 0.11 0.49
4 -1 27 -0.39 0.50
4 1 27 -0.13 0.54
-4 -1 27 -0.21 0.41
-4 1 27 -0.21 0.37
0 2 -27 2.53 0.76
1 2 -27 -0.14 0.61
-1 2 -27 0.30 0.57
2 2 -27 12.28 1.37
-2 2 -27 12.94 1.41
3 2 -27 0.46 0.51
-3 2 -27 0.36 0.45
-4 2 -27 12.20 1.18
0 3 -27 -0.25 0.47
1 3 -27 9.82 1.14
1 3 -27 10.79 1.17
-1 3 -27 8.50 1.11
2 3 -27 0.52 0.46
-2 3 -27 0.11 0.38
0 0 28 5.25 1.00
0 0 -28 6.06 1.06
1 0 28 2.87 0.83
-1 0 28 3.36 0.81
-1 0 -28 4.16 0.92
2 0 28 34.66 2.56
-2 0 28 37.15 2.50
-2 0 -28 38.87 2.55
3 0 28 2.61 0.73
-3 0 28 1.81 0.54
-3 0 -28 1.56 0.63
-4 0 28 0.69 0.38
0 -1 28 0.51 0.51
0 1 28 -0.13 0.50
0 -1 -28 0.37 0.55
0 1 -28 0.12 0.54
1 -1 28 0.51 0.50
1 1 28 1.55 0.62
-1 -1 28 1.32 0.55
-1 1 28 2.15 0.61
-1 -1 -28 1.93 0.66
-1 1 -28 1.81 0.69
1 -1 -28 1.96 0.66
1 1 -28 1.59 0.65
2 -1 28 0.48 0.45
2 1 28 0.75 0.50
-2 -1 28 0.87 0.45
-2 1 28 1.08 0.49
-2 -1 -28 1.79 0.64
-2 1 -28 0.67 0.56
-2 1 -28 1.81 0.56
3 -1 28 0.11 0.39
3 1 28 0.56 0.46
-3 -1 28 0.47 0.37
-3 1 28 0.19 0.33
-3 -1 -28 0.20 0.42
-3 1 -28 0.69 0.50
0 2 -28 20.80 1.72
1 2 -28 -0.11 0.44
-1 2 -28 0.12 0.44
2 2 -28 21.78 1.62
2 2 -28 19.67 1.58
-2 2 -28 20.42 1.61
0 0 29 -0.10 0.36
0 0 -29 0.10 0.48
1 0 29 0.61 0.43
-1 0 29 0.10 0.36
-1 0 -29 -0.20 0.46
1 0 -29 0.50 0.46
0 1 -29 0.89 0.44
0 0 0 0.00 0.00
TITL exp_310_ni+phba+mea in Pbca
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 1.54184 11.081183 7.632580 23.798586 90.0000 90.0000 90.0000
ZERR 9.00 0.000216 0.000174 0.000488 0.0000 0.0000 0.0000
LATT 1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O
UNIT 99.00 90.00 9.00 9.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 55422
_shelx_res_file
;
TITL exp_310_ni+phba+mea_a.res in Pbca
i.res
created by SHELXL-2018/3 at 11:05:50 on 15-May-2022
REM Old TITL exp_310_ni+phba+mea_a.res in Pbca
REM SHELXT solution in Pbca: R1 0.109, Rweak 0.023, Alpha 0.012
REM 0.558 for 329 systematic absences, Orientation as input
REM Formula found by SHELXT: C14 O14 Mn
CELL 1.54184 11.081183 7.63258 23.798586 90 90 90
ZERR 4 0.000216 0.000174 0.000488 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Ni O
UNIT 56 104 4 56
L.S. 4 0 0
PLAN 5
SIZE 0.15 0.2 0.18
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM
REM
REM
WGHT 0.060100 0.479900
FVAR 0.34882
NI1 3 0.500000 0.500000 0.500000 10.50000 0.02385 0.04007 =
0.02715 -0.00160 0.00049 0.00122
O5 4 0.320839 0.562257 0.481300 11.00000 0.02592 0.05353 =
0.03332 -0.00230 0.00066 0.00168
O7 4 0.545360 0.536735 0.417404 11.00000 0.03145 0.05873 =
0.02933 -0.00144 0.00129 0.00006
O6 4 0.461619 0.240976 0.485588 11.00000 0.04786 0.04026 =
0.03759 -0.00435 0.00524 -0.00212
O2 4 0.043071 0.529342 0.580572 11.00000 0.03916 0.05342 =
0.03573 -0.00529 -0.00592 0.00082
O4 4 0.312426 0.649030 0.909855 11.00000 0.03515 0.05839 =
0.05045 -0.00720 -0.00405 -0.00199
O3 4 0.125310 0.578892 0.843903 11.00000 0.03904 0.10386 =
0.03173 0.00513 -0.00083 -0.01468
O1 4 0.235438 0.610202 0.583326 11.00000 0.03323 0.08400 =
0.03426 -0.00113 0.00553 0.00529
C1 1 0.133659 0.575284 0.669954 11.00000 0.02872 0.04022 =
0.03443 -0.00114 0.00042 0.00227
C2 1 0.227906 0.650414 0.700193 11.00000 0.02988 0.04408 =
0.03826 0.00082 0.00219 -0.00540
AFIX 43
H2 2 0.293016 0.698597 0.680979 11.00000 -1.20000
AFIX 0
C4 1 0.130266 0.579803 0.786793 11.00000 0.03095 0.05083 =
0.03328 0.00266 -0.00006 0.00099
C7 1 0.138091 0.570523 0.607132 11.00000 0.03203 0.04412 =
0.03652 -0.00309 -0.00031 0.00753
C3 1 0.226512 0.654710 0.758025 11.00000 0.03184 0.04765 =
0.03846 -0.00100 -0.00244 -0.00711
AFIX 43
H3A 2 0.289389 0.707250 0.777671 11.00000 -1.20000
AFIX 0
C6 1 0.037984 0.501388 0.699490 11.00000 0.02790 0.04864 =
0.03919 -0.00091 -0.00302 -0.00374
AFIX 43
H6 2 -0.025565 0.450481 0.679870 11.00000 -1.20000
AFIX 0
C5 1 0.036003 0.502529 0.757559 11.00000 0.02828 0.05709 =
0.03996 0.00488 0.00201 -0.00592
AFIX 43
H5 2 -0.028059 0.451858 0.776878 11.00000 -1.20000
AFIX 0
H6A 2 0.455595 0.183363 0.514048 11.00000 0.05688
H5A 2 0.286092 0.485625 0.459737 11.00000 0.06487
H7A 2 0.494370 0.496054 0.394770 11.00000 0.06074
H6B 2 0.498505 0.183465 0.464222 11.00000 0.07479
H7B 2 0.618565 0.487287 0.407964 11.00000 0.08149
H5B 2 0.281940 0.585561 0.514453 11.00000 0.08530
H4A 2 0.318201 0.738963 0.928740 11.00000 0.08791
H4B 2 0.384702 0.609395 0.905554 11.00000 0.08463
H3 2 0.191638 0.619259 0.857293 11.00000 0.08338
HKLF 4
REM exp_310_ni+phba+mea_a.res in Pbca
REM wR2 = 0.1012, GooF = S = 1.050, Restrained GooF = 1.050 for all data
REM R1 = 0.0338 for 1656 Fo > 4sig(Fo) and 0.0400 for all 1949 data
REM 169 parameters refined using 0 restraints
END
WGHT 0.0601 0.4799
REM Highest difference peak 0.247, deepest hole -0.432, 1-sigma level 0.055
Q1 1 0.1344 0.5796 0.6447 11.00000 0.05 0.25
Q2 1 0.4733 0.3428 0.4860 11.00000 0.05 0.22
Q3 1 0.4982 0.3552 0.5003 11.00000 0.05 0.18
Q4 1 0.0444 0.5092 0.5412 11.00000 0.05 0.16
Q5 1 0.0462 0.4241 0.5808 11.00000 0.05 0.16
;
_shelx_res_checksum 23546
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.500000 0.500000 0.500000 0.03036(17) Uani d 1 . .
O O5 0.32084(12) 0.5623(2) 0.48130(6) 0.0376(3) Uani d 1 . .
O O7 0.54536(14) 0.5367(2) 0.41740(6) 0.0398(3) Uani d 1 . .
O O6 0.46162(15) 0.2410(2) 0.48559(7) 0.0419(3) Uani d 1 . .
O O2 0.04307(14) 0.5293(2) 0.58057(6) 0.0428(4) Uani d 1 . .
O O4 0.31243(14) 0.6490(2) 0.90986(7) 0.0480(4) Uani d 1 . .
O O3 0.12531(15) 0.5789(3) 0.84390(6) 0.0582(5) Uani d 1 . .
O O1 0.23544(12) 0.6102(2) 0.58333(6) 0.0505(4) Uani d 1 . .
C C1 0.13366(16) 0.5753(3) 0.66995(8) 0.0345(4) Uani d 1 . .
C C2 0.22791(16) 0.6504(3) 0.70019(8) 0.0374(4) Uani d 1 . .
H H2 0.293016 0.698597 0.680979 0.045 Uiso calc 1 . .
C C4 0.13027(16) 0.5798(3) 0.78679(8) 0.0384(4) Uani d 1 . .
C C7 0.13809(17) 0.5705(3) 0.60713(8) 0.0376(4) Uani d 1 . .
C C3 0.22651(17) 0.6547(3) 0.75802(8) 0.0393(4) Uani d 1 . .
H H3A 0.289389 0.707250 0.777671 0.047 Uiso calc 1 . .
C C6 0.03798(18) 0.5014(3) 0.69949(9) 0.0386(4) Uani d 1 . .
H H6 -0.025565 0.450481 0.679870 0.046 Uiso calc 1 . .
C C5 0.03600(19) 0.5025(3) 0.75756(9) 0.0418(5) Uani d 1 . .
H H5 -0.028059 0.451858 0.776878 0.050 Uiso calc 1 . .
H H6A 0.456(3) 0.183(4) 0.5140(13) 0.057(8) Uiso d 1 . .
H H5A 0.286(3) 0.486(4) 0.4597(12) 0.065(9) Uiso d 1 . .
H H7A 0.494(3) 0.496(3) 0.3948(15) 0.061(10) Uiso d 1 . .
H H6B 0.499(3) 0.183(5) 0.4642(15) 0.075(10) Uiso d 1 . .
H H7B 0.619(4) 0.487(4) 0.4080(14) 0.081(10) Uiso d 1 . .
H H5B 0.282(3) 0.586(4) 0.5145(15) 0.085(10) Uiso d 1 . .
H H4A 0.318(3) 0.739(5) 0.9287(14) 0.088(11) Uiso d 1 . .
H H4B 0.385(3) 0.609(4) 0.9056(13) 0.085(10) Uiso d 1 . .
H H3 0.192(3) 0.619(4) 0.8573(14) 0.083(10) 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
Ni1 0.0238(3) 0.0401(3) 0.0272(3) 0.00122(16) 0.00049(15) -0.00160(16)
O5 0.0259(6) 0.0535(9) 0.0333(7) 0.0017(6) 0.0007(5) -0.0023(6)
O7 0.0314(7) 0.0587(9) 0.0293(7) 0.0001(7) 0.0013(5) -0.0014(6)
O6 0.0479(8) 0.0403(8) 0.0376(8) -0.0021(7) 0.0052(7) -0.0043(7)
O2 0.0392(8) 0.0534(9) 0.0357(8) 0.0008(6) -0.0059(6) -0.0053(6)
O4 0.0352(8) 0.0584(10) 0.0505(9) -0.0020(7) -0.0041(6) -0.0072(7)
O3 0.0390(8) 0.1039(14) 0.0317(7) -0.0147(9) -0.0008(6) 0.0051(8)
O1 0.0332(7) 0.0840(11) 0.0343(7) 0.0053(7) 0.0055(5) -0.0011(7)
C1 0.0287(8) 0.0402(10) 0.0344(10) 0.0023(8) 0.0004(7) -0.0011(7)
C2 0.0299(9) 0.0441(11) 0.0383(10) -0.0054(8) 0.0022(7) 0.0008(8)
C4 0.0309(9) 0.0508(11) 0.0333(9) 0.0010(9) -0.0001(7) 0.0027(8)
C7 0.0320(9) 0.0441(11) 0.0365(10) 0.0075(8) -0.0003(7) -0.0031(8)
C3 0.0318(9) 0.0477(11) 0.0385(10) -0.0071(8) -0.0024(7) -0.0010(8)
C6 0.0279(9) 0.0486(12) 0.0392(10) -0.0037(8) -0.0030(8) -0.0009(8)
C5 0.0283(9) 0.0571(13) 0.0400(11) -0.0059(8) 0.0020(8) 0.0049(8)
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'
Ni Ni -3.0029 0.5091 '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
O5 Ni1 O5 . 5_666 180.00(8) ?
O7 Ni1 O5 . 5_666 90.14(6) ?
O7 Ni1 O5 . . 89.86(6) ?
O7 Ni1 O5 5_666 . 90.14(6) ?
O7 Ni1 O5 5_666 5_666 89.86(6) ?
O7 Ni1 O7 . 5_666 180.0 ?
O7 Ni1 O6 5_666 5_666 91.28(7) ?
O7 Ni1 O6 5_666 . 88.72(7) ?
O7 Ni1 O6 . . 91.28(7) ?
O7 Ni1 O6 . 5_666 88.72(7) ?
O6 Ni1 O5 . 5_666 90.77(6) ?
O6 Ni1 O5 . . 89.23(6) ?
O6 Ni1 O5 5_666 . 90.77(6) ?
O6 Ni1 O5 5_666 5_666 89.23(6) ?
O6 Ni1 O6 . 5_666 180.0 ?
Ni1 O5 H5A . . 113(2) ?
Ni1 O5 H5B . . 108(2) ?
H5A O5 H5B . . 116(3) ?
Ni1 O7 H7A . . 114(2) ?
Ni1 O7 H7B . . 113(2) ?
H7A O7 H7B . . 107(3) ?
Ni1 O6 H6A . . 114(2) ?
Ni1 O6 H6B . . 123(2) ?
H6A O6 H6B . . 106(4) ?
H4A O4 H4B . . 107(3) ?
C4 O3 H3 . . 110(2) ?
C2 C1 C7 . . 120.13(17) ?
C6 C1 C2 . . 118.52(17) ?
C6 C1 C7 . . 121.33(17) ?
C1 C2 H2 . . 119.4 ?
C3 C2 C1 . . 121.21(17) ?
C3 C2 H2 . . 119.4 ?
O3 C4 C3 . . 121.67(18) ?
O3 C4 C5 . . 117.95(17) ?
C5 C4 C3 . . 120.37(18) ?
O2 C7 C1 . . 118.49(17) ?
O1 C7 O2 . . 123.26(18) ?
O1 C7 C1 . . 118.24(17) ?
C2 C3 C4 . . 119.41(17) ?
C2 C3 H3A . . 120.3 ?
C4 C3 H3A . . 120.3 ?
C1 C6 H6 . . 119.5 ?
C5 C6 C1 . . 120.97(18) ?
C5 C6 H6 . . 119.5 ?
C4 C5 H5 . . 120.3 ?
C6 C5 C4 . . 119.50(18) ?
C6 C5 H5 . . 120.3 ?
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
Ni1 O5 5_666 2.0893(13) ?
Ni1 O5 . 2.0893(13) ?
Ni1 O7 . 2.0482(13) ?
Ni1 O7 5_666 2.0483(13) ?
Ni1 O6 5_666 2.0511(15) ?
Ni1 O6 . 2.0511(15) ?
O5 H5A . 0.87(3) ?
O5 H5B . 0.92(4) ?
O7 H7A . 0.84(3) ?
O7 H7B . 0.92(4) ?
O6 H6A . 0.81(3) ?
O6 H6B . 0.79(3) ?
O2 C7 . 1.268(2) ?
O4 H4A . 0.82(4) ?
O4 H4B . 0.86(4) ?
O3 C4 . 1.360(2) ?
O3 H3 . 0.86(4) ?
O1 C7 . 1.256(2) ?
C1 C2 . 1.392(3) ?
C1 C7 . 1.496(3) ?
C1 C6 . 1.391(3) ?
C2 H2 . 0.9300 ?
C2 C3 . 1.377(3) ?
C4 C3 . 1.390(3) ?
C4 C5 . 1.387(3) ?
C3 H3A . 0.9300 ?
C6 H6 . 0.9300 ?
C6 C5 . 1.382(3) ?
C5 H5 . 0.9300 ?
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
O3 H3 O4 . 0.86(3) 1.84(3) 2.655(2) 157(3) yes
O4 H4A O5 7_576 0.82(4) 1.97(4) 2.785(2) 173(4) yes
O4 H4B O2 6_657 0.87(3) 1.88(3) 2.724(2) 163(3) yes
O5 H5A O4 2_564 0.87(3) 1.91(3) 2.770(2) 169(3) yes
O5 H5B O1 . 0.92(4) 1.73(4) 2.632(2) 168(3) yes
O6 H6A O2 8_655 0.81(3) 1.97(3) 2.779(2) 174(3) yes
O6 H6B O2 4_556 0.79(4) 2.00(4) 2.748(2) 157(4) yes
O7 H7A O3 2_564 0.84(3) 1.88(3) 2.723(2) 176(3) yes
O7 H7B O1 5_666 0.93(4) 1.79(4) 2.675(2) 159(3) 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
O3 C4 C3 C2 . . . . 179.3(2) ?
O3 C4 C5 C6 . . . . 179.88(19) ?
C1 C2 C3 C4 . . . . 1.2(3) ?
C1 C6 C5 C4 . . . . 0.6(3) ?
C2 C1 C7 O2 . . . . -168.06(18) ?
C2 C1 C7 O1 . . . . 10.9(3) ?
C2 C1 C6 C5 . . . . 0.1(3) ?
C7 C1 C2 C3 . . . . -179.30(18) ?
C7 C1 C6 C5 . . . . 178.40(18) ?
C3 C4 C5 C6 . . . . -0.4(3) ?
C6 C1 C2 C3 . . . . -1.0(3) ?
C6 C1 C7 O2 . . . . 13.7(3) ?
C6 C1 C7 O1 . . . . -167.37(19) ?
C5 C4 C3 C2 . . . . -0.5(3) ?
_cod_database_fobs_code 2244104