#------------------------------------------------------------------------------
#$Date: 2025-03-04 21:47:03 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298196 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249680.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_7249680
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            'C16 H11 Cl8 O13 Y'
_chemical_formula_weight         783.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5640(6)
_cell_length_b                   18.5537(9)
_cell_length_c                   12.1650(6)
_cell_measurement_reflns_used    8549
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.3864
_cell_measurement_theta_min      2.6666
_cell_volume                     2610.1(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         2.075
_exptl_absorpt_coefficient_mu    3.117
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6513
_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    1.995
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 2293 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5978
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0265
_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)+(0.0199P)²+0.8998P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0529
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5414
_reflns_number_total             5978
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00966e2.cif
_cod_data_source_block           shelx_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7249676--7249681.cif.'
_cod_database_code               7249680
_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, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
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 0.38679(3) 0.56790(2) 0.47148(3) 0.01030(8) Uani 1 1 d . . . . .
Cl1 Cl 0.54122(11) 0.79408(6) 0.42293(10) 0.0317(3) Uani 1 1 d . . . . .
Cl2 Cl 0.55809(12) 0.95809(6) 0.47194(13) 0.0443(3) Uani 1 1 d . . . . .
Cl3 Cl 0.41356(14) 1.02493(6) 0.66159(11) 0.0432(4) Uani 1 1 d . . . . .
Cl4 Cl 0.25068(11) 0.92963(6) 0.80078(10) 0.0301(3) Uani 1 1 d . . . . .
Cl5 Cl 0.54262(8) 0.30737(5) 0.53247(8) 0.0182(2) Uani 1 1 d . . . . .
Cl6 Cl 0.49422(8) 0.14891(5) 0.46683(11) 0.0236(2) Uani 1 1 d . . . . .
Cl7 Cl 0.33115(11) 0.11461(6) 0.27140(11) 0.0308(3) Uani 1 1 d . . . . .
Cl8 Cl 0.21337(12) 0.23922(7) 0.14251(11) 0.0377(3) Uani 1 1 d . . . . .
O1 O 0.4334(2) 0.66182(15) 0.6282(2) 0.0179(6) Uani 1 1 d . . . . .
O2 O 0.3336(2) 0.69004(13) 0.4806(2) 0.0150(5) Uani 1 1 d . . . . .
O3 O 0.2035(2) 0.71915(16) 0.7145(2) 0.0193(6) Uani 1 1 d . . . . .
O4 O 0.2808(3) 0.77635(16) 0.8586(2) 0.0237(7) Uani 1 1 d . . . . .
H4 H 0.244157 0.745222 0.894617 0.028 Uiso 1 1 calc R U . . .
O5 O 0.3149(2) 0.44906(14) 0.4466(2) 0.0159(6) Uani 1 1 d . . . . .
O6 O 0.4944(2) 0.45980(14) 0.3905(2) 0.0162(6) Uani 1 1 d . . . . .
O7 O 0.1550(3) 0.39835(17) 0.2316(2) 0.0236(7) Uani 1 1 d . . . . .
O8 O 0.3288(2) 0.43576(15) 0.1792(2) 0.0156(6) Uani 1 1 d . . . . .
O9 O 0.4539(2) 0.50487(15) 0.6255(2) 0.0157(6) Uani 1 1 d D . . . .
H9A H 0.496969 0.528382 0.667052 0.019 Uiso 1 1 d DG U . . .
H9B H 0.419996 0.470229 0.655630 0.019 Uiso 1 1 d DG U . . .
O10 O 0.2267(3) 0.56081(16) 0.5910(3) 0.0163(7) Uani 1 1 d D . . . .
H10A H 0.169240 0.586235 0.585668 0.020 Uiso 1 1 d DG U . . .
H10B H 0.219002 0.519305 0.621724 0.020 Uiso 1 1 d DG U . . .
O11 O 0.2211(3) 0.57800(18) 0.3504(2) 0.0171(7) Uani 1 1 d D . . . .
H11A H 0.153476 0.571389 0.360211 0.021 Uiso 1 1 d DG U . . .
H11B H 0.215315 0.586817 0.286329 0.021 Uiso 1 1 d DG U . . .
O12 O 0.4370(2) 0.61446(15) 0.2980(2) 0.0147(6) Uani 1 1 d D . . . .
H12A H 0.510329 0.620148 0.282395 0.018 Uiso 1 1 d DG U . . .
H12B H 0.395040 0.650727 0.273568 0.018 Uiso 1 1 d DG U . . .
O13 O 0.5832(2) 0.60006(14) 0.4778(3) 0.0155(5) Uani 1 1 d D . . . .
H13A H 0.600743 0.605461 0.549856 0.019 Uiso 1 1 d DG U . . .
H13B H 0.632919 0.586662 0.426055 0.019 Uiso 1 1 d DG U . . .
C1 C 0.3868(3) 0.7074(2) 0.5693(3) 0.0123(8) Uani 1 1 d . . . . .
C2 C 0.3942(3) 0.7866(2) 0.5948(3) 0.0141(8) Uani 1 1 d . . . . .
C3 C 0.4622(4) 0.8311(2) 0.5296(3) 0.0196(9) Uani 1 1 d . . . . .
C4 C 0.4705(4) 0.9044(2) 0.5502(4) 0.0232(10) Uani 1 1 d . . . . .
C5 C 0.4063(4) 0.9341(2) 0.6359(4) 0.0245(10) Uani 1 1 d . . . . .
C6 C 0.3362(4) 0.8901(2) 0.7012(3) 0.0182(9) Uani 1 1 d . . . . .
C7 C 0.3331(3) 0.8162(2) 0.6830(3) 0.0134(8) Uani 1 1 d . . . . .
C8 C 0.2642(3) 0.7659(2) 0.7538(3) 0.0132(8) Uani 1 1 d . . . . .
C9 C 0.4048(3) 0.4224(2) 0.4047(3) 0.0116(8) Uani 1 1 d . . . . .
C10 C 0.3969(3) 0.3447(2) 0.3687(3) 0.0125(8) Uani 1 1 d . . . . .
C11 C 0.4524(3) 0.2897(2) 0.4229(3) 0.0133(8) Uani 1 1 d . . . . .
C12 C 0.4313(4) 0.2178(2) 0.3940(3) 0.0146(8) Uani 1 1 d . . . . .
C13 C 0.3577(4) 0.2025(2) 0.3076(3) 0.0163(8) Uani 1 1 d . . . . .
C14 C 0.3023(4) 0.2587(2) 0.2519(3) 0.0171(9) Uani 1 1 d . . . . .
C15 C 0.3205(3) 0.3293(2) 0.2830(3) 0.0123(8) Uani 1 1 d . . . . .
C16 C 0.2616(4) 0.3922(2) 0.2262(4) 0.0143(8) Uani 1 1 d . . . . .
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'
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 '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'
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
O9 Y1 O13 77.30(10) . . ?
O9 Y1 O2 122.06(10) . . ?
O13 Y1 O2 90.38(9) . . ?
O9 Y1 O12 145.04(10) . . ?
O13 Y1 O12 72.42(10) . . ?
O2 Y1 O12 75.69(10) . . ?
O9 Y1 O10 74.85(10) . . ?
O13 Y1 O10 138.83(11) . . ?
O2 Y1 O10 79.59(10) . . ?
O12 Y1 O10 140.11(10) . . ?
O9 Y1 O5 75.79(10) . . ?
O13 Y1 O5 125.33(9) . . ?
O2 Y1 O5 143.99(9) . . ?
O12 Y1 O5 108.21(10) . . ?
O10 Y1 O5 75.64(10) . . ?
O9 Y1 O11 141.90(10) . . ?
O13 Y1 O11 139.86(10) . . ?
O2 Y1 O11 75.35(10) . . ?
O12 Y1 O11 67.76(10) . . ?
O10 Y1 O11 76.02(9) . . ?
O5 Y1 O11 73.59(10) . . ?
O9 Y1 O6 75.83(10) . . ?
O13 Y1 O6 75.02(9) . . ?
O2 Y1 O6 154.34(9) . . ?
O12 Y1 O6 79.78(9) . . ?
O10 Y1 O6 125.15(10) . . ?
O5 Y1 O6 52.66(9) . . ?
O11 Y1 O6 102.20(10) . . ?
O9 Y1 O1 71.57(9) . . ?
O13 Y1 O1 67.11(10) . . ?
O2 Y1 O1 51.90(9) . . ?
O12 Y1 O1 110.81(10) . . ?
O10 Y1 O1 75.61(10) . . ?
O5 Y1 O1 140.95(9) . . ?
O11 Y1 O1 123.33(10) . . ?
O6 Y1 O1 134.16(9) . . ?
O9 Y1 C9 74.25(10) . . ?
O13 Y1 C9 100.41(10) . . ?
O2 Y1 C9 162.43(10) . . ?
O12 Y1 C9 94.27(10) . . ?
O10 Y1 C9 100.49(11) . . ?
O5 Y1 C9 26.24(10) . . ?
O11 Y1 C9 87.56(11) . . ?
O6 Y1 C9 26.43(10) . . ?
O1 Y1 C9 145.42(9) . . ?
O9 Y1 C1 96.86(11) . . ?
O13 Y1 C1 75.85(10) . . ?
O2 Y1 C1 26.44(10) . . ?
O12 Y1 C1 92.36(10) . . ?
O10 Y1 C1 78.05(11) . . ?
O5 Y1 C1 153.69(10) . . ?
O11 Y1 C1 100.58(11) . . ?
O6 Y1 C1 150.85(10) . . ?
O1 Y1 C1 25.59(10) . . ?
C9 Y1 C1 171.01(11) . . ?
C1 O1 Y1 86.8(2) . . ?
C1 O2 Y1 99.0(2) . . ?
C9 O5 Y1 97.3(2) . . ?
C9 O6 Y1 88.8(2) . . ?
O1 C1 O2 121.8(4) . . ?
O1 C1 C2 121.7(3) . . ?
O2 C1 C2 116.4(3) . . ?
O1 C1 Y1 67.6(2) . . ?
O2 C1 Y1 54.60(19) . . ?
C2 C1 Y1 166.8(3) . . ?
C3 C2 C7 119.5(4) . . ?
C3 C2 C1 119.7(3) . . ?
C7 C2 C1 120.8(3) . . ?
C2 C3 C4 121.2(4) . . ?
C2 C3 Cl1 119.5(3) . . ?
C4 C3 Cl1 119.3(3) . . ?
C3 C4 C5 119.2(4) . . ?
C3 C4 Cl2 120.8(3) . . ?
C5 C4 Cl2 120.1(3) . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 Cl3 119.9(3) . . ?
C6 C5 Cl3 119.9(3) . . ?
C7 C6 C5 120.0(4) . . ?
C7 C6 Cl4 121.1(3) . . ?
C5 C6 Cl4 118.8(3) . . ?
C6 C7 C2 119.8(4) . . ?
C6 C7 C8 122.4(4) . . ?
C2 C7 C8 117.8(4) . . ?
O3 C8 O4 125.3(4) . . ?
O3 C8 C7 121.7(3) . . ?
O4 C8 C7 113.0(3) . . ?
O6 C9 O5 121.2(3) . . ?
O6 C9 C10 122.5(3) . . ?
O5 C9 C10 116.2(3) . . ?
O6 C9 Y1 64.8(2) . . ?
O5 C9 Y1 56.47(19) . . ?
C10 C9 Y1 172.3(3) . . ?
C11 C10 C15 120.2(4) . . ?
C11 C10 C9 122.8(4) . . ?
C15 C10 C9 116.8(3) . . ?
C10 C11 C12 120.4(4) . . ?
C10 C11 Cl5 120.8(3) . . ?
C12 C11 Cl5 118.7(3) . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 Cl6 120.1(3) . . ?
C11 C12 Cl6 120.4(3) . . ?
C12 C13 C14 119.9(4) . . ?
C12 C13 Cl7 119.9(3) . . ?
C14 C13 Cl7 120.1(3) . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 Cl8 120.2(3) . . ?
C13 C14 Cl8 119.5(3) . . ?
C14 C15 C10 119.7(4) . . ?
C14 C15 C16 122.5(4) . . ?
C10 C15 C16 117.8(3) . . ?
O7 C16 O8 125.4(4) . . ?
O7 C16 C15 119.5(4) . . ?
O8 C16 C15 115.1(4) . . ?
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 O9 2.341(3) . ?
Y1 O13 2.349(2) . ?
Y1 O2 2.351(2) . ?
Y1 O12 2.353(3) . ?
Y1 O10 2.358(3) . ?
Y1 O5 2.376(3) . ?
Y1 O11 2.424(3) . ?
Y1 O6 2.558(3) . ?
Y1 O1 2.639(3) . ?
Y1 C9 2.827(4) . ?
Y1 C1 2.849(4) . ?
Cl1 C3 1.729(4) . ?
Cl2 C4 1.711(4) . ?
Cl3 C5 1.716(4) . ?
Cl4 C6 1.727(4) . ?
Cl5 C11 1.724(4) . ?
Cl6 C12 1.716(4) . ?
Cl7 C13 1.717(4) . ?
Cl8 C14 1.720(4) . ?
O1 C1 1.232(5) . ?
O2 C1 1.284(5) . ?
O3 C8 1.214(5) . ?
O4 C8 1.303(4) . ?
O5 C9 1.260(4) . ?
O6 C9 1.259(5) . ?
O7 C16 1.240(5) . ?
O8 C16 1.258(5) . ?
C1 C2 1.505(5) . ?
C2 C3 1.389(6) . ?
C2 C7 1.396(5) . ?
C3 C4 1.386(6) . ?
C4 C5 1.393(6) . ?
C5 C6 1.399(6) . ?
C6 C7 1.389(6) . ?
C7 C8 1.500(5) . ?
C9 C10 1.509(5) . ?
C10 C11 1.374(5) . ?
C10 C15 1.396(5) . ?
C11 C12 1.402(5) . ?
C12 C13 1.382(6) . ?
C13 C14 1.398(6) . ?
C14 C15 1.381(6) . ?
C15 C16 1.517(5) . ?
