#------------------------------------------------------------------------------
#$Date: 2025-03-04 21:47:03 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249677.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_7249677
loop_
_publ_author_name
'Ngom, Fallou'
'Blais, Chloé'
'Badiane, Insa'
'Hénaff, Christine'
'Camara, Magatte'
'Daiguebonne, Carole'
'Guillou, Olivier'
_publ_section_title
;
 Influence of halogens on the crystal packing of
 3,4,5,6-tetra-chloro-phthalate-based lanthanide coordination compounds
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              210
_journal_page_last               225
_journal_paper_doi               10.1039/D4CE00966E
_journal_volume                  27
_journal_year                    2025
_chemical_formula_sum            'C8 H10 Cl4 O8 Y'
_chemical_formula_weight         464.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-10-28 deposited with the CCDC.	2024-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.615(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7595(6)
_cell_length_b                   6.7789(5)
_cell_length_c                   11.8297(9)
_cell_measurement_reflns_used    2620
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.29
_cell_measurement_theta_min      2.34
_cell_volume                     699.07(9)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2741
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.768
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.969
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.955
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1697
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0538P)²+2.9045P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1491
_reflns_number_total             1697
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00966e2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7249676--7249681.cif.'
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7249677
_shelx_shelxl_version_number     2018/3
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
Y1 Y 0.37470(6) 0.750000 0.95702(5) 0.01777(19) Uani 1 2 d S T P . .
Cl1 Cl 0.63919(19) 0.250000 0.6835(2) 0.0462(5) Uani 1 2 d S T P . .
Cl2 Cl 0.5217(2) 0.250000 0.42593(17) 0.0371(4) Uani 1 2 d S T P . .
Cl3 Cl 0.1680(2) 0.250000 0.35374(14) 0.0389(5) Uani 1 2 d S T P . .
Cl4 Cl -0.06071(18) 0.250000 0.53805(15) 0.0349(4) Uani 1 2 d S T P . .
O1 O 0.4281(6) 0.4087(6) 0.8968(3) 0.0591(14) Uani 1 1 d . . . . .
O2 O 0.0372(5) 0.4114(7) 0.8196(4) 0.0496(11) Uani 1 1 d . . . . .
H2 H -0.012173 0.473862 0.766630 0.059 Uiso 0.5 1 calc R U P . .
O3 O 0.6047(9) 0.750000 0.8607(6) 0.0570(18) Uani 1 2 d DS T P . .
H3B H 0.551(12) 0.750000 0.798(5) 0.068 Uiso 1 2 d DS U P . .
O4 O 0.2058(8) 0.750000 0.7908(6) 0.0559(19) Uani 1 2 d DS T P . .
H4A H 0.173(6) 0.863(5) 0.776(6) 0.067 Uiso 1 1 d D U . . .
H4B H 0.299(4) 0.750000 0.783(10) 0.067 Uiso 1 2 d DS U P . .
O5 O 0.1998(6) 0.5397(9) 1.0459(4) 0.0585(13) Uani 1 1 d D . . . .
H5A H 0.134(7) 0.574(12) 1.088(6) 0.070 Uiso 1 1 d D U . . .
C1 C 0.3430(7) 0.250000 0.7238(5) 0.0201(12) Uani 1 2 d S T P . .
C2 C 0.4456(7) 0.250000 0.6414(6) 0.0247(14) Uani 1 2 d S T P . .
C3 C 0.3923(7) 0.250000 0.5264(6) 0.0246(14) Uani 1 2 d S T P . .
C4 C 0.2354(8) 0.250000 0.4940(5) 0.0259(14) Uani 1 2 d S T P . .
C5 C 0.1342(7) 0.250000 0.5781(5) 0.0226(13) Uani 1 2 d S T P . .
C6 C 0.1869(7) 0.250000 0.6920(5) 0.0210(13) Uani 1 2 d S T P . .
C7 C 0.4050(8) 0.250000 0.8479(6) 0.0275(15) Uani 1 2 d S T P . .
C8 C 0.0762(8) 0.250000 0.7841(6) 0.0269(15) Uani 1 2 d S T P . .
H5B H 0.193(18) 0.415(3) 1.048(14) 0.29(11) Uiso 1 1 d D . . . .
H3A H 0.694(6) 0.750000 0.842(12) 0.6(4) Uiso 1 2 d DS . P . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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'
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
O4 Y1 O5 89.4(2) . 4_575 ?
O4 Y1 O5 89.4(2) . . ?
O5 Y1 O5 72.6(2) 4_575 . ?
O4 Y1 O3 95.3(3) . . ?
O5 Y1 O3 143.46(12) 4_575 . ?
O5 Y1 O3 143.46(12) . . ?
O4 Y1 O1 83.13(12) . 4_575 ?
O5 Y1 O1 73.66(18) 4_575 4_575 ?
O5 Y1 O1 145.48(18) . 4_575 ?
O3 Y1 O1 70.99(13) . 4_575 ?
O4 Y1 O1 83.13(12) . . ?
O5 Y1 O1 145.48(18) 4_575 . ?
O5 Y1 O1 73.66(18) . . ?
O3 Y1 O1 70.99(13) . . ?
O1 Y1 O1 137.9(2) 4_575 . ?
O4 Y1 O1 153.71(12) . 2_657 ?
O5 Y1 O1 82.68(18) 4_575 2_657 ?
O5 Y1 O1 111.74(18) . 2_657 ?
O3 Y1 O1 77.2(2) . 2_657 ?
O1 Y1 O1 70.60(14) 4_575 2_657 ?
O1 Y1 O1 116.91(11) . 2_657 ?
O4 Y1 O1 153.71(12) . 3_667 ?
O5 Y1 O1 111.74(18) 4_575 3_667 ?
O5 Y1 O1 82.68(18) . 3_667 ?
O3 Y1 O1 77.2(2) . 3_667 ?
O1 Y1 O1 116.92(11) 4_575 3_667 ?
O1 Y1 O1 70.60(14) . 3_667 ?
O1 Y1 O1 49.72(19) 2_657 3_667 ?
O4 Y1 C7 176.8(3) . 3_667 ?
O5 Y1 C7 93.20(18) 4_575 3_667 ?
O5 Y1 C7 93.20(18) . 3_667 ?
O3 Y1 C7 81.5(2) . 3_667 ?
O1 Y1 C7 95.76(11) 4_575 3_667 ?
O1 Y1 C7 95.76(11) . 3_667 ?
O1 Y1 C7 25.44(10) 2_657 3_667 ?
O1 Y1 C7 25.44(10) 3_667 3_667 ?
O4 Y1 H3B 76.2(10) . . ?
O5 Y1 H3B 141.3(4) 4_575 . ?
O5 Y1 H3B 141.3(4) . . ?
O3 Y1 H3B 19.1(10) . . ?
O1 Y1 H3B 69.08(13) 4_575 . ?
O1 Y1 H3B 69.08(12) . . ?
O1 Y1 H3B 94.5(9) 2_657 . ?
O1 Y1 H3B 94.5(9) 3_667 . ?
C7 Y1 H3B 100.6(10) 3_667 . ?
O4 Y1 H4B 20.7(7) . . ?
O5 Y1 H4B 105.9(6) 4_575 . ?
O5 Y1 H4B 105.9(6) . . ?
O3 Y1 H4B 74.6(7) . . ?
O1 Y1 H4B 76.6(2) 4_575 . ?
O1 Y1 H4B 76.6(2) . . ?
O1 Y1 H4B 142.2(5) 2_657 . ?
O1 Y1 H4B 142.2(5) 3_667 . ?
C7 Y1 H4B 156.1(7) 3_667 . ?
H3B Y1 H4B 55.5(12) . . ?
C7 O1 Y1 157.7(5) . . ?
C7 O1 Y1 91.1(4) . 3_667 ?
Y1 O1 Y1 109.40(14) . 3_667 ?
C8 O2 H2 109.5 . . ?
Y1 O3 H3B 90(9) . . ?
Y1 O3 H3A 167(10) . . ?
H3B O3 H3A 103(4) . . ?
Y1 O4 H4A 111(5) . . ?
Y1 O4 H4B 63(8) . . ?
H4A O4 H4B 108(4) . . ?
Y1 O4 H4A 111(5) . 4_575 ?
H4A O4 H4A 134(9) . 4_575 ?
H4B O4 H4A 108(4) . 4_575 ?
Y1 O5 H5A 127(6) . . ?
Y1 O5 H5B 131(7) . . ?
H5A O5 H5B 102(4) . . ?
C6 C1 C2 120.0(6) . . ?
C6 C1 C7 121.0(6) . . ?
C2 C1 C7 119.0(6) . . ?
C1 C2 C3 120.4(6) . . ?
C1 C2 Cl1 118.9(5) . . ?
C3 C2 Cl1 120.7(5) . . ?
C4 C3 C2 119.8(6) . . ?
C4 C3 Cl2 120.6(5) . . ?
C2 C3 Cl2 119.5(5) . . ?
C3 C4 C5 118.9(6) . . ?
C3 C4 Cl3 120.5(5) . . ?
C5 C4 Cl3 120.6(5) . . ?
C6 C5 C4 121.4(6) . . ?
C6 C5 Cl4 119.6(5) . . ?
C4 C5 Cl4 119.0(5) . . ?
C5 C6 C1 119.5(6) . . ?
C5 C6 C8 121.4(6) . . ?
C1 C6 C8 119.1(6) . . ?
O1 C7 O1 122.2(6) . 4_565 ?
O1 C7 C1 118.9(3) . . ?
O1 C7 C1 118.9(3) 4_565 . ?
O1 C7 Y1 63.5(3) . 3_667 ?
O1 C7 Y1 63.5(3) 4_565 3_667 ?
C1 C7 Y1 158.7(5) . 3_667 ?
O2 C8 O2 125.3(7) . 4_565 ?
O2 C8 C6 117.3(3) . . ?
O2 C8 C6 117.3(3) 4_565 . ?
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
Y1 O4 2.342(6) . ?
Y1 O5 2.408(5) 4_575 ?
Y1 O5 2.409(5) . ?
Y1 O3 2.410(8) . ?
Y1 O1 2.479(5) 4_575 ?
Y1 O1 2.479(5) . ?
Y1 O1 2.559(5) 2_657 ?
Y1 O1 2.559(4) 3_667 ?
Y1 C7 2.859(7) 3_667 ?
Y1 H3B 2.55(12) . ?
Y1 H4B 2.10(11) . ?
Cl1 C2 1.720(6) . ?
Cl2 C3 1.721(6) . ?
Cl3 C4 1.705(7) . ?
Cl4 C5 1.727(6) . ?
O1 C7 1.229(5) . ?
O2 C8 1.232(5) . ?
O2 H2 0.8400 . ?
O3 H3B 0.83(2) . ?
O3 H3A 0.84(2) . ?
O4 H4A 0.83(2) . ?
O4 H4B 0.83(2) . ?
O4 H4A 0.83(2) 4_575 ?
O5 H5A 0.83(2) . ?
O5 H5B 0.84(2) . ?
C1 C6 1.383(9) . ?
C1 C2 1.390(9) . ?
C1 C7 1.515(9) . ?
C2 C3 1.394(9) . ?
C3 C4 1.390(9) . ?
C4 C5 1.396(9) . ?
C5 C6 1.381(8) . ?
C6 C8 1.528(9) . ?
