#------------------------------------------------------------------------------
#$Date: 2024-02-04 12:37:03 +0100 (Sun 04 de Feb de 2024) $
#$Revision: 289439 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/79/7247929.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7247929
loop_
_publ_author_name
'Meekel, Emily G.'
'Nicholas, Thomas C.'
'Slater, Ben'
'Goodwin, Andrew L.'
_publ_section_title
;
 Torsional flexibility in zinc-benzenedicarboxylate metal-organic
 frameworks.
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              673
_journal_page_last               680
_journal_paper_doi               10.1039/d3ce01078c
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C8 H3 I O4 Zn'
_chemical_formula_sum            'C8 H3 I O4 Zn'
_chemical_formula_weight         355.37
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-10-19 deposited with the CCDC.	2023-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   28.5799(4)
_cell_length_b                   28.5799(4)
_cell_length_c                   8.09130(10)
_cell_measurement_reflns_used    5860
_cell_measurement_temperature    290.15
_cell_measurement_theta_max      75.7230
_cell_measurement_theta_min      5.3480
_cell_volume                     5723.61(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      290.15
_diffrn_detector_area_resol_mean 13.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger 1M'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7511
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.989
_diffrn_reflns_theta_min         5.362
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    21.677
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.51889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.83a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       rod
_exptl_crystal_F_000             2988
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.257
_refine_diff_density_min         -2.492
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1405
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0666
_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/[σ²(Fo²)+(0.1427P)²+57.1873P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2117
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1371
_reflns_number_total             1405
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01078c1.cif
_cod_data_source_block           em-01-98_1_30s
_cod_depositor_comments
'Adding full bibliography for 7247925--7247930.cif.'
_cod_original_cell_volume        5723.61(18)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7247929
_shelx_shelxl_version_number     2019/1
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 C5, C4, C2, C1, C3, C2_$1, C4_$1, H4_$1, H4, H3, C1_$1
 with sigma of 0.1
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_file
;
TITL em-01-98_1_30s_a.res in R-3m
    em-01-98_1_30s.res
    created by SHELXL-2019/1 at 14:54:58 on 29-May-2023
REM Old TITL EM-01-98_1_30s in R-3m
REM SHELXT solution in R-3m: R1 0.276, Rweak 0.053, Alpha 0.057
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C4 O2 Zn
CELL 1.54184 28.5799 28.5799 8.0913 90 90 120
ZERR 18 0.0004 0.0004 0.0001 0 0 0
LATT 3
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM +Y,+X,-Z
SYMM -Y+X,-Y,-Z
SYMM -X,-X+Y,-Z
SFAC C H I O Zn
UNIT 144 54 18 72 18
EQIV $1 1-Y,1-X,+Z
FLAT C5 C4 C2 C1 C3 C2_$1 C4_$1 H4_$1 H4 H3 C1_$1

L.S. 4 0 0
PLAN  2
TEMP 17
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\EM-01-98_1_30s.hkl">
REM </olex2.extras>

WGHT    0.142700   57.187305
FVAR       0.10792
I1    3    0.562362    0.437638    0.123805    10.50000    0.10208    0.10208 =
         0.05309   -0.02689    0.02689    0.03423
ZN1   5    0.622941    0.622941    1.000000    10.50000    0.03057    0.03057 =
         0.02730   -0.00229    0.00229    0.01686
O2    4    0.649979    0.598519    0.601313    11.00000    0.04523    0.03738 =
         0.05008   -0.00295   -0.00108    0.00516
O1    4    0.592997    0.573983    0.814902    11.00000    0.04804    0.04718 =
         0.04136   -0.01561   -0.00404    0.01598
C2    1    0.571371    0.512969    0.596757    11.00000    0.03472    0.03257 =
         0.02890   -0.00262    0.00094    0.01277
C1    1    0.608001    0.565668    0.677881    11.00000    0.03638    0.03322 =
         0.03388   -0.00387   -0.00360    0.01427
C3    1    0.523273    0.476727    0.674007    10.50000    0.03247    0.03247 =
         0.02808   -0.00239    0.00239    0.01194
AFIX  43
H3    2    0.515290    0.484710    0.778051    10.50000   -1.20000
AFIX   0
C5    1    0.546574    0.453426    0.362881    10.50000    0.05108    0.05108 =
         0.02710   -0.00916    0.00916    0.02544
C4    1    0.583127    0.501135    0.439231    11.00000    0.03500    0.04162 =
         0.03743   -0.00092    0.01230    0.01397
AFIX  43
H4    2    0.615236    0.525183    0.386636    11.00000   -1.20000
AFIX   0
HKLF 4




REM  em-01-98_1_30s_a.res in R-3m
REM wR2 = 0.2121, GooF = S = 1.118, Restrained GooF = 1.117 for all data
REM R1 = 0.0666 for 1371 Fo > 4sig(Fo) and 0.0670 for all 1405 data
REM 69 parameters refined using 8 restraints

END

WGHT      0.1425     55.3684

REM Highest difference peak  3.257,  deepest hole -2.492,  1-sigma level  0.210
Q1    1   0.5792  0.4208  0.1975  10.50000  0.05    3.26
Q2    1   0.6193  0.3807  0.5554  10.50000  0.05    1.44
;
_shelx_res_checksum              95035
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -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'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+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'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, 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'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+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'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.56236(3) 0.43764(3) 0.12381(11) 0.0932(5) Uani 1 2 d S T P . .
Zn1 Zn 0.62294(3) 0.62294(3) 1.000000 0.0288(4) Uani 1 2 d S T P . .
O2 O 0.6500(2) 0.59852(19) 0.6013(7) 0.0511(12) Uani 1 1 d . . . . .
O1 O 0.59300(19) 0.5740(2) 0.8149(6) 0.0490(12) Uani 1 1 d . . . . .
C2 C 0.5714(2) 0.5130(2) 0.5968(7) 0.0339(11) Uani 1 1 d . . . . .
C1 C 0.6080(2) 0.5657(2) 0.6779(7) 0.0359(12) Uani 1 1 d . . . . .
C3 C 0.52327(16) 0.47673(16) 0.6740(10) 0.0329(15) Uani 1 2 d S T P . .
H3 H 0.515290 0.484710 0.778051 0.039 Uiso 1 2 calc R U P . .
C5 C 0.54657(17) 0.45343(17) 0.3629(10) 0.0431(19) Uani 1 2 d S T P . .
C4 C 0.5831(2) 0.5011(2) 0.4392(8) 0.0403(13) Uani 1 1 d . . . . .
H4 H 0.615236 0.525183 0.386636 0.048 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.1021(7) 0.1021(7) 0.0531(6) -0.0269(3) 0.0269(3) 0.0342(6)
Zn1 0.0306(5) 0.0306(5) 0.0273(6) -0.00229(17) 0.00229(17) 0.0169(4)
O2 0.045(2) 0.037(2) 0.050(3) -0.003(2) -0.001(2) 0.0052(19)
O1 0.048(2) 0.047(2) 0.041(3) -0.016(2) -0.004(2) 0.016(2)
C2 0.035(3) 0.033(3) 0.029(3) -0.003(2) 0.001(2) 0.013(2)
C1 0.036(3) 0.033(3) 0.034(3) -0.004(2) -0.004(2) 0.014(2)
C3 0.032(3) 0.032(3) 0.028(4) -0.0024(15) 0.0024(15) 0.012(3)
C5 0.051(3) 0.051(3) 0.027(4) -0.0092(18) 0.0092(18) 0.025(4)
C4 0.035(3) 0.042(3) 0.037(3) -0.001(2) 0.012(2) 0.014(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'
I I -0.3257 6.8362 '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'
Zn Zn -1.5491 0.6778 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O2 133.9(4) 18_656 9_565 ?
O2 Zn1 O1 103.2(2) 9_565 4_557 ?
O2 Zn1 O1 103.2(2) 18_656 4_557 ?
O2 Zn1 O1 103.2(2) 9_565 . ?
O2 Zn1 O1 103.2(2) 18_656 . ?
O1 Zn1 O1 108.6(3) 4_557 . ?
C1 O2 Zn1 131.3(5) . 14_654 ?
C1 O1 Zn1 138.8(4) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 C4 119.8(5) . . ?
C4 C2 C1 120.8(5) . . ?
O2 C1 C2 117.7(5) . . ?
O1 C1 O2 125.7(6) . . ?
O1 C1 C2 116.6(5) . . ?
C2 C3 C2 120.4(7) 22_665 . ?
C2 C3 H3 119.8 22_665 . ?
C2 C3 H3 119.8 . . ?
C4 C5 I1 119.3(4) 22_665 . ?
C4 C5 I1 119.3(4) . . ?
C4 C5 C4 121.3(8) . 22_665 ?
C2 C4 H4 120.3 . . ?
C5 C4 C2 119.4(5) . . ?
C5 C4 H4 120.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 C5 2.086(8) . ?
Zn1 O2 1.921(5) 18_656 ?
Zn1 O2 1.921(5) 9_565 ?
Zn1 O1 1.933(5) 4_557 ?
Zn1 O1 1.933(5) . ?
O2 C1 1.256(8) . ?
O1 C1 1.254(8) . ?
C2 C1 1.489(8) . ?
C2 C3 1.389(7) . ?
C2 C4 1.402(8) . ?
C3 H3 0.9300 . ?
C5 C4 1.381(7) . ?
C5 C4 1.381(7) 22_665 ?
C4 H4 0.9300 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I1 C5 C4 C2 177.0(5) . . . . ?
Zn1 O2 C1 O1 9.2(11) 14_654 . . . ?
Zn1 O2 C1 C2 -173.5(4) 14_654 . . . ?
Zn1 O1 C1 O2 -17.3(11) . . . . ?
Zn1 O1 C1 C2 165.4(5) . . . . ?
C1 C2 C3 C2 176.4(5) . . . 22_665 ?
C1 C2 C4 C5 -175.7(6) . . . . ?
C3 C2 C1 O2 -176.9(6) . . . . ?
C3 C2 C1 O1 0.7(8) . . . . ?
C3 C2 C4 C5 0.0(7) . . . . ?
C4 C2 C1 O2 -1.1(8) . . . . ?
C4 C2 C1 O1 176.4(5) . . . . ?
C4 C2 C3 C2 0.6(11) . . . 22_665 ?
C4 C5 C4 C2 -0.6(9) 22_665 . . . ?
