#------------------------------------------------------------------------------
#$Date: 2025-04-05 14:45:22 +0300 (Sat, 05 Apr 2025) $
#$Revision: 299192 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/30/07/2300754.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_2300754
loop_
_publ_author_name
'Biehler, Erik'
'Pagola, Silvina'
'Stam, Daniel'
'Merkelbach, Johannes'
'Jandl, Christian'
'Abdel-Fattah, Tarek M'
_publ_section_title
;
 A comparison of microcrystal electron diffraction and X-ray powder
 diffraction for the structural analysis of metal-organic frameworks.
;
_journal_coeditor_code           TE5145SUP1
_journal_issue                   'Pt 2'
_journal_name_full               'Journal of applied crystallography'
_journal_page_first              398
_journal_page_last               411
_journal_paper_doi               10.1107/S1600576724012068
_journal_volume                  58
_journal_year                    2025
_chemical_formula_moiety         'C8 H8 Ni O6, H2 O'
_chemical_formula_sum            'C8 H10 Ni O7'
_chemical_formula_weight         276.9
_chemical_name_common            'nickel terephthalate trihydrate'
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_method           'Jana2020 1.3.51'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   20.31(5)
_cell_length_b                   22.85(5)
_cell_length_c                   6.226(14)
_cell_measurement_reflns_used    1737
_cell_measurement_temperature    293
_cell_measurement_theta_max      1.0291
_cell_measurement_theta_min      0.04084
_cell_volume                     2889(12)
_diffrn_ambient_temperature      293
_diffrn_detector                 'Dectris QUADRO'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.84
_diffrn_measured_fraction_theta_max 0.81
_diffrn_measurement_device       'ELDICO ED-1'
_diffrn_measurement_device_type  'electron diffractometer'
_diffrn_measurement_method       'continuous rotation 3D ED'
_diffrn_radiation_probe          electron
_diffrn_radiation_source         LaB~6~
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02851
_diffrn_reflns_av_unetI/netI     0.1665
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            34947
_diffrn_reflns_theta_full        0.53
_diffrn_reflns_theta_max         0.9
_diffrn_reflns_theta_min         0.05
_exptl_absorpt_coefficient_mu    0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.9098
_exptl_crystal_description       plate
_exptl_crystal_F_000             549.32
_exptl_crystal_size_max          0.003
_exptl_crystal_size_mid          0.0015
_exptl_crystal_size_min          0.0002
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    0.0000
_refine_ls_goodness_of_fit_ref   1.7456
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    36
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6918
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.2070
_refine_ls_R_factor_gt           0.1157
_refine_ls_shift/su_max          0.0096
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.02P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.2274
_refine_ls_wR_factor_ref         0.2467
_reflns_number_gt                2038
_reflns_number_total             6918
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            te5145.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 2300754--2300756.cif.'
_cod_original_sg_symbol_Hall     '-P -2xab;-2yc;-2zabc'
_cod_original_formula_sum        'C8 H10 Ni1 O7'
_cod_database_code               2300754
_jana_m40_file
;
   42    0    0    1    0
 1.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 0.000000 0.000000 0.000000                                 000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 1.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 0.000000 0.000000 0.000000                                 000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 1.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 0.000000 0.000000 0.000000                                 000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000      000000
Ni1       3  1     0.500000 0.000000 0.000000 0.500000
 0.008951 0.000000 0.000000 0.000000 0.000000 0.000000      0000100000
O1        4  1     1.000000 0.031092 0.386329 0.603693
 0.028482 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
C1        1  1     0.500000 0.000000 0.360964 0.750000
 0.016085 0.000000 0.000000 0.000000 0.000000 0.000000      0010100000
Ni2       3  1     1.000000 0.165988 0.498237-0.096892
 0.005042 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
O2        4  1     1.000000-0.004480 0.084184 0.567851
 0.011526 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
C2        1  1     0.500000 0.000000 0.296112 0.750000
 0.009180 0.000000 0.000000 0.000000 0.000000 0.000000      0010100000
C3        1  1     1.000000 0.011334 0.265119 0.943710
 0.017381 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H3        2  1     1.000000 0.018227 0.288419 1.092960
 0.020857 0.000000 0.000000 0.000000 0.000000 0.000000      0000000000
C4        1  1     1.000000 0.013443 0.204646 0.938976
 0.011526 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H4        2  1     1.000000 0.025578 0.180479 1.082711
 0.013831 0.000000 0.000000 0.000000 0.000000 0.000000      0000000000
C5        1  1     0.500000 0.000000 0.175113 0.750000
 0.011526 0.000000 0.000000 0.000000 0.000000 0.000000      0010000000
C6        1  1     0.500000 0.000000 0.109162 0.750000
 0.011526 0.000000 0.000000 0.000000 0.000000 0.000000      0010000000
O11       4  1     1.000000 0.168399 0.413668-0.024669
 0.013950 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
O12       4  1     1.000000 0.162631 0.417668 0.333141
 0.015140 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
O13       4  1     1.000000 0.201821 0.112116 0.056666
 0.021510 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
O14       4  1     1.000000 0.129524 0.114263 0.335179
 0.024081 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
C21       1  1     1.000000 0.165137 0.326392 0.167396
 0.004694 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
C22       1  1     1.000000 0.145185 0.296229 0.359775
 0.014926 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H22       2  1     1.000000 0.130931 0.320778 0.500538
 0.017911 0.000000 0.000000 0.000000 0.000000 0.000000      0000000000
C23       1  1     1.000000 0.144356 0.236640 0.363581
 0.020671 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H23       2  1     1.000000 0.126540 0.214095 0.504542
 0.024805 0.000000 0.000000 0.000000 0.000000 0.000000      0000000000
C24       1  1     1.000000 0.166689 0.203851 0.183991
 0.009066 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
C25       1  1     1.000000 0.187208 0.233282-0.001848
 0.013653 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H25       2  1     1.000000 0.204067 0.208878-0.139861
 0.016384 0.000000 0.000000 0.000000 0.000000 0.000000      0000000000
C26       1  1     1.000000 0.185727 0.293618-0.007300
 0.014667 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H26       2  1     1.000000 0.201050 0.315932-0.151829
 0.017601 0.000000 0.000000 0.000000 0.000000 0.000000      0000000000
C27       1  1     1.000000 0.166316 0.390897 0.160863
 0.008344 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
C28       1  1     1.000000 0.167676 0.139575 0.190541
 0.016200 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
O31       4  1     1.000000 0.167540 0.059196 0.694815
 0.016090 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H31A      2  1     1.000000 0.161269 0.081750 0.549415
 0.019308 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
H31B      2  1     1.000000 0.177656 0.082960 0.833138
 0.019308 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O32       4  1     1.000000 0.067666-0.016478 0.753032
 0.007631 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H32A      2  1     1.000000 0.107986 0.012528 0.755067
 0.009157 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
H32B      2  1     1.000000 0.091473-0.057458 0.750109
 0.009157 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O33       4  1     1.000000 0.097156 0.483957-0.343594
 0.007813 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H33A      2  1     1.000000 0.066378 0.521774-0.319767
 0.009376 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
H33B      2  1     1.000000 0.067398 0.446709-0.352648
 0.009376 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O34       4  1     1.000000 0.235075 0.516072 0.150211
 0.009799 0.000000 0.000000 0.000000 0.000000 0.000000      0111100000
H34A      2  1     1.000000 0.257889 0.555005 0.103300
 0.011759 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
H34B      2  1     1.000000 0.275029 0.486128 0.158469
 0.011759 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
O41       4  1     0.500000 0.000000 0.444062 0.250000
 0.023155 0.000000 0.000000 0.000000 0.000000 0.000000      0010100000
H41       2  1     1.000000 0.008067 0.418606 0.383589
 0.027787 0.000000 0.000000 0.000000 0.000000 0.000000      0111000000
--------------------------   s.u. block   --------------------------------------
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
Ni1                0.000000 0.000000 0.000000 0.000000
 0.000444 0.000000 0.000000 0.000000 0.000000 0.000000
O1                 0.000000 0.000231 0.000217 0.000717
 0.001174 0.000000 0.000000 0.000000 0.000000 0.000000
C1                 0.000000 0.000000 0.000299 0.000000
 0.001539 0.000000 0.000000 0.000000 0.000000 0.000000
Ni2                0.000000 0.000081 0.000059 0.000187
 0.000317 0.000000 0.000000 0.000000 0.000000 0.000000
O2                 0.000000 0.000196 0.000171 0.000534
 0.000582 0.000000 0.000000 0.000000 0.000000 0.000000
C2                 0.000000 0.000000 0.000278 0.000000
 0.001425 0.000000 0.000000 0.000000 0.000000 0.000000
C3                 0.000000 0.000208 0.000209 0.000673
 0.001185 0.000000 0.000000 0.000000 0.000000 0.000000
H3                 0.000000-0.100000-0.100000-0.100000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
C4                 0.000000 0.000194 0.000200 0.000646
 0.000582 0.000000 0.000000 0.000000 0.000000 0.000000
H4                 0.000000-0.100000-0.100000-0.100000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
C5                 0.000000 0.000000 0.000291 0.000000
 0.000582 0.000000 0.000000 0.000000 0.000000 0.000000
C6                 0.000000 0.000000 0.000288 0.000000
 0.000582 0.000000 0.000000 0.000000 0.000000 0.000000
O11                0.000000 0.000212 0.000154 0.000573
 0.000863 0.000000 0.000000 0.000000 0.000000 0.000000
O12                0.000000 0.000237 0.000142 0.000606
 0.000865 0.000000 0.000000 0.000000 0.000000 0.000000
O13                0.000000 0.000200 0.000192 0.000641
 0.001054 0.000000 0.000000 0.000000 0.000000 0.000000
O14                0.000000 0.000203 0.000189 0.000665
 0.001064 0.000000 0.000000 0.000000 0.000000 0.000000
C21                0.000000 0.000238 0.000163 0.000600
 0.000845 0.000000 0.000000 0.000000 0.000000 0.000000
C22                0.000000 0.000192 0.000202 0.000708
 0.001148 0.000000 0.000000 0.000000 0.000000 0.000000
H22                0.000000-0.100000-0.100000-0.100000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
C23                0.000000 0.000205 0.000217 0.000736
 0.001225 0.000000 0.000000 0.000000 0.000000 0.000000
H23                0.000000-0.100000-0.100000-0.100000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
C24                0.000000 0.000251 0.000171 0.000623
 0.000945 0.000000 0.000000 0.000000 0.000000 0.000000
C25                0.000000 0.000197 0.000208 0.000712
 0.001095 0.000000 0.000000 0.000000 0.000000 0.000000
H25                0.000000-0.100000-0.100000-0.100000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
C26                0.000000 0.000190 0.000208 0.000715
 0.001118 0.000000 0.000000 0.000000 0.000000 0.000000
H26                0.000000-0.100000-0.100000-0.100000
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
C27                0.000000 0.000251 0.000170 0.000651
 0.000924 0.000000 0.000000 0.000000 0.000000 0.000000
C28                0.000000 0.000274 0.000179 0.000692
 0.001035 0.000000 0.000000 0.000000 0.000000 0.000000
O31                0.000000 0.000233 0.000152 0.000646
 0.000894 0.000000 0.000000 0.000000 0.000000 0.000000
H31A               0.000000 0.001206 0.000805 0.002003
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
H31B               0.000000 0.001098 0.000779 0.002333
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
O32                0.000000 0.000169 0.000153 0.000647
 0.000784 0.000000 0.000000 0.000000 0.000000 0.000000
H32A               0.000000 0.000701 0.000678 0.003150
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
H32B               0.000000 0.000810 0.000525 0.003331
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
O33                0.000000 0.000186 0.000179 0.000557
 0.000869 0.000000 0.000000 0.000000 0.000000 0.000000
H33A               0.000000 0.000675 0.000484 0.002894
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
H33B               0.000000 0.000673 0.000469 0.003130
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
O34                0.000000 0.000199 0.000185 0.000565
 0.000935 0.000000 0.000000 0.000000 0.000000 0.000000
H34A               0.000000 0.000920 0.000601 0.003175
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
H34B               0.000000 0.000793 0.000738 0.002968
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
O41                0.000000 0.000000 0.000280 0.000000
 0.001436 0.000000 0.000000 0.000000 0.000000 0.000000
H41                0.000000 0.001170 0.000916 0.002652
 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000
--------------------------   Saved points   ------------------------------------
    0
--------------------------   Critical points   ---------------------------------
    0
--------------------------   Fourier maxima   ----------------------------------
    1    1    3
Max1      1  1     1.000000 0.000000-0.000000 0.000000      000  0  0  0
     0.93     0.50
Max2      1  1     1.000000 0.666763 0.003730 0.099508      000  0  0  0
     0.85     0.40
Max3      1  1     1.000000 0.931883 0.016103 0.231205      000  0  0  0
     0.37     0.22
Max4      1  1     1.000000 0.333816 0.000807 0.156478      000  0  0  0
     0.52     0.21
Max5      1  1     1.000000 0.400284 0.015991 0.162085      000  0  0  0
     0.36     0.21
Max6      1  1     1.000000 0.267141 0.015235 0.144576      000  0  0  0
     0.30     0.16
Max7      1  1     1.000000 0.668300 0.083836 0.031126      000  0  0  0
     0.24     0.13
Max8      1  1     1.000000 0.000696 0.134721 0.250000      000  0  0  0
     0.16     0.13
Max9      1  1     1.000000 0.761696 0.485939 0.071526      000  0  0  0
     0.21     0.13
Max10     1  1     1.000000 0.333532 0.434066 0.215823      000  0  0  0
     0.26     0.12
--------------------------   Fourier minima   ----------------------------------
    1    1    3
Min1      1  1     1.000000 0.696062 0.025802 0.230017      000  0  0  0
     0.34     0.22
Min2      1  1     1.000000 0.034210 0.000324 0.154944      000  0  0  0
     0.34     0.21
Min3      1  1     1.000000 0.364847 0.024013 0.061528      000  0  0  0
     0.34     0.20
Min4      1  1     1.000000 0.531327 0.525351 0.114320      000  0  0  0
     0.31     0.19
Min5      1  1     1.000000 0.302253 0.016528 0.023063      000  0  0  0
     0.32     0.19
--------------------------------------------------------------------------------
;
_jana_m50_file
;
Version Jana2020
title
cell 20.30817 22.84715 6.22579 90 90 90
esdcell 0.05 0.05 0.014 0 0 0
spgroup Pbcn 60 3
lattice P
symmetry x y z
symmetry -x+1/2 -y+1/2 z+1/2
symmetry -x y -z+1/2
symmetry x+1/2 -y+1/2 -z
symmetry -x -y -z
symmetry x+1/2 y+1/2 -z+1/2
symmetry x -y z+1/2
symmetry -x+1/2 y+1/2 z
unitsnumb 12
atlist C8 H10 Ni O7
formtab -62
atom C atradius 0.77 color 128073041
atom H atradius 0.46 color 255204204
atom Ni atradius 1.25 color 183187189
atom O atradius 0.74 color 254003000
roundmethod 1
end
*******************************************************************************
refine
  cycles 20 damp 10 convlim 0.01 uisolim 0
  restric C4 12 C5 C6 O2
  distfix = 0.0099999998 O31 H31A; O31 H31B; O32 H32A; O32 H32B; O33 H33A; O33 H
  &33B; O34 H34A; O34 H34B; O41 H41
  anglefix 109 0.1000000015 H33A O33 H33B
  keep hydro triang C3 2 1 C2 C4 1.08 H3
  keep ADP riding C3 1.2 H3
  keep hydro triang C4 2 1 C3 C5 1.08 H4
  keep ADP riding C4 1.2 H4
  keep hydro triang C22 2 1 C21 C23 1.08 H22
  keep ADP riding C22 1.2 H22
  keep hydro triang C23 2 1 C22 C24 1.08 H23
  keep ADP riding C23 1.2 H23
  keep hydro triang C25 2 1 C24 C26 1.08 H25
  keep ADP riding C25 1.2 H25
  keep hydro triang C26 2 1 C25 C21 1.08 H26
  keep ADP riding C26 1.2 H26
  keep ADP riding O31 1.2 H31A H31B
  keep ADP riding O32 1.2 H32A H32B
  keep ADP riding O33 1.2 H33A H33B
  keep ADP riding O34 1.2 H34A H34B
  keep ADP riding O41 1.2 H41
end refine
fourier
end fourier
dist
end dist
contour
end contour
;
