#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:37:03 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289439 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/79/7247927.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_7247927
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 Cl O4 Zn'
_chemical_formula_sum            'C8 H3 Cl O4 Zn'
_chemical_formula_weight         263.92
_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                   28.4445(5)
_cell_length_b                   28.4445(5)
_cell_length_c                   7.82240(10)
_cell_measurement_reflns_used    7360
_cell_measurement_temperature    295.15
_cell_measurement_theta_max      73.0110
_cell_measurement_theta_min      5.3780
_cell_volume                     5481.09(15)
_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      295.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Eiger 1M'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24893
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.850
_diffrn_reflns_theta_min         5.387
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.751
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.63000
_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            colorless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       rod
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1357
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0492
_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)+(0.1028P)²+12.5876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1253
_reflns_number_total             1357
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01078c1.cif
_cod_data_source_block           em-01-78_1
_cod_depositor_comments
'Adding full bibliography for 7247925--7247930.cif.'
_cod_original_cell_volume        5481.1(2)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               7247927
_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
 C2_$1, C3, C2, C4, C5, C4_$1, C1, C1_$1, Cl1
 with sigma of 0.1
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_shelx_res_file
;
TITL em-01-78_1_a.res in R-3m
    em-01-78_1.res
    created by SHELXL-2019/1 at 14:44:18 on 29-May-2023
REM Old TITL EM-01-78_1 in R-3m
REM SHELXT solution in R-3m: R1 0.134, Rweak 0.007, Alpha 0.027
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 O4 Cl Zn
CELL 1.54184 28.4445 28.4445 7.8224 90 90 120
ZERR 18 0.0005 0.0005 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 Cl O Zn
UNIT 144 54 18 72 18
EQIV $1 1+Y-X,+Y,+Z
FLAT C2_$1 C3 C2 C4 C5 C4_$1 C1 C1_$1 Cl1

L.S. 4 0 0
PLAN  2
TEMP 22
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
OMIT 0 2 1
OMIT -1 1 1
REM <olex2.extras>
REM <HklSrc "%.\\EM-01-78_1.hkl">
REM </olex2.extras>

WGHT    0.102800   12.587600
FVAR       0.16783
ZN1   5    0.711108    0.666667    0.166667    10.50000    0.03707    0.03312 =
         0.03534    0.00392    0.00196    0.01656
CL1   3    0.776020    0.552040    1.041413    10.50000    0.10012    0.16542 =
         0.05854    0.05766    0.02883    0.08271
O2    4    0.681774    0.613123    0.579628    11.00000    0.04819    0.07264 =
         0.05226   -0.00206   -0.00205    0.04002
O1    4    0.738220    0.643380    0.356462    11.00000    0.05319    0.06576 =
         0.04930    0.01402   -0.00312    0.03372
C3    1    0.807808    0.615616    0.502949    10.50000    0.04309    0.04703 =
         0.03223    0.00541    0.00271    0.02351
AFIX  43
H3    2    0.814610    0.629221    0.392048    10.50000   -1.20000
AFIX   0
C1    1    0.723584    0.621306    0.499981    11.00000    0.04357    0.04353 =
         0.04131   -0.00230   -0.00576    0.02395
C2    1    0.760603    0.605434    0.585946    11.00000    0.03957    0.04606 =
         0.04021    0.00290    0.00047    0.02306
C5    1    0.787472    0.574943    0.829926    10.50000    0.05589    0.06728 =
         0.04269    0.02013    0.01006    0.03364
C4    1    0.749996    0.584784    0.750792    11.00000    0.04217    0.05903 =
         0.04769    0.01314    0.00961    0.02727
AFIX  43
H4    2    0.718271    0.577733    0.806707    11.00000   -1.20000
AFIX   0
HKLF 4




REM  em-01-78_1_a.res in R-3m
REM wR2 = 0.1576, GooF = S = 1.124, Restrained GooF = 1.125 for all data
REM R1 = 0.0492 for 1253 Fo > 4sig(Fo) and 0.0515 for all 1357 data
REM 69 parameters refined using 6 restraints

END

WGHT      0.1025     12.6640

REM Highest difference peak  0.937,  deepest hole -0.765,  1-sigma level  0.135
Q1    1   0.7589  0.5179  0.9665  10.50000  0.05    0.94
Q2    1   0.8185  0.4851  1.3333  10.50000  0.05    0.79
;
_shelx_res_checksum              21962
_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
Zn1 Zn 0.71111(2) 0.666667 0.166667 0.0356(3) Uani 1 2 d S T P . .
Cl1 Cl 0.77602(6) 0.55204(11) 1.0414(2) 0.1008(8) Uani 1 2 d S T P . .
O2 O 0.68177(10) 0.61312(12) 0.5796(3) 0.0533(6) Uani 1 1 d . . . . .
O1 O 0.73822(11) 0.64338(11) 0.3565(3) 0.0543(7) Uani 1 1 d . . . . .
C3 C 0.80781(8) 0.61562(17) 0.5029(5) 0.0403(9) Uani 1 2 d S T P . .
H3 H 0.814610 0.629221 0.392048 0.048 Uiso 1 2 calc R U P . .
C1 C 0.72358(14) 0.62131(13) 0.5000(4) 0.0418(7) Uani 1 1 d . . . . .
C2 C 0.76060(13) 0.60543(12) 0.5859(4) 0.0412(7) Uani 1 1 d . . . . .
C5 C 0.78747(13) 0.5749(3) 0.8299(7) 0.0540(12) Uani 1 2 d S T P . .
C4 C 0.75000(14) 0.58478(16) 0.7508(5) 0.0488(8) Uani 1 1 d . . . . .
H4 H 0.718271 0.577733 0.806707 0.059 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
Zn1 0.0371(3) 0.0331(4) 0.0353(4) 0.00392(19) 0.00196(10) 0.01656(18)
Cl1 0.1001(9) 0.165(2) 0.0585(9) 0.0577(12) 0.0288(6) 0.0827(11)
O2 0.0482(13) 0.0726(17) 0.0523(14) -0.0021(12) -0.0020(11) 0.0400(13)
O1 0.0532(14) 0.0658(16) 0.0493(14) 0.0140(11) -0.0031(10) 0.0337(13)
C3 0.0431(17) 0.047(2) 0.032(2) 0.0054(17) 0.0027(8) 0.0235(12)
C1 0.0436(17) 0.0435(16) 0.0413(16) -0.0023(13) -0.0058(12) 0.0240(13)
C2 0.0396(16) 0.0461(17) 0.0402(16) 0.0029(13) 0.0005(12) 0.0231(13)
C5 0.056(2) 0.067(3) 0.043(3) 0.020(2) 0.0101(11) 0.0336(16)
C4 0.0422(17) 0.059(2) 0.0477(18) 0.0131(15) 0.0096(14) 0.0273(16)
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'
Cl Cl 0.3639 0.7018 '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 136.59(18) 14_654 18_655 ?
O1 Zn1 O2 102.87(12) 11_565 18_655 ?
O1 Zn1 O2 102.86(12) . 14_654 ?
O1 Zn1 O2 101.45(12) 11_565 14_654 ?
O1 Zn1 O2 101.45(12) . 18_655 ?
O1 Zn1 O1 110.59(17) 11_565 . ?
C1 O2 Zn1 128.7(2) . 9_565 ?
C1 O1 Zn1 140.4(2) . . ?
C2 C3 H3 120.2 . . ?
C2 C3 H3 120.2 23_655 . ?
C2 C3 C2 119.7(4) . 23_655 ?
O2 C1 C2 117.7(3) . . ?
O1 C1 O2 125.7(3) . . ?
O1 C1 C2 116.5(3) . . ?
C3 C2 C1 118.7(3) . . ?
C3 C2 C4 120.5(3) . . ?
C4 C2 C1 120.6(3) . . ?
C4 C5 Cl1 118.8(2) 23_655 . ?
C4 C5 Cl1 118.8(2) . . ?
C4 C5 C4 122.3(5) . 23_655 ?
C2 C4 H4 120.7 . . ?
C5 C4 C2 118.5(3) . . ?
C5 C4 H4 120.7 . . ?
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
Zn1 O2 1.940(2) 14_654 ?
Zn1 O2 1.940(2) 18_655 ?
Zn1 O1 1.936(3) 11_565 ?
Zn1 O1 1.936(3) . ?
Cl1 C5 1.748(5) . ?
O2 C1 1.257(4) . ?
O1 C1 1.252(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.385(4) 23_655 ?
C3 C2 1.385(4) . ?
C1 C2 1.497(4) . ?
C2 C4 1.386(5) . ?
C5 C4 1.377(4) 23_655 ?
C5 C4 1.377(4) . ?
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
Zn1 O2 C1 O1 8.9(5) 9_565 . . . ?
Zn1 O2 C1 C2 -173.7(2) 9_565 . . . ?
Zn1 O1 C1 O2 -11.2(6) . . . . ?
Zn1 O1 C1 C2 171.4(3) . . . . ?
Cl1 C5 C4 C2 176.9(4) . . . . ?
O2 C1 C2 C3 -178.0(3) . . . . ?
O2 C1 C2 C4 -2.9(5) . . . . ?
O1 C1 C2 C3 -0.3(4) . . . . ?
O1 C1 C2 C4 174.8(3) . . . . ?
C3 C2 C4 C5 0.3(6) . . . . ?
C1 C2 C4 C5 -174.7(4) . . . . ?
C2 C3 C2 C1 174.6(2) 23_655 . . . ?
C2 C3 C2 C4 -0.5(6) 23_655 . . . ?
C4 C5 C4 C2 -0.2(9) 23_655 . . . ?
