Four series of lanthanide coordination polymers based on the tetrabromobenzene-1,4-dicarboxylate ligand: structural diversity and multifunctional properties
Jiajaroen, Suwadee; Dungkeaw, Winya; Kielar, Filip; Sukwattanasinitt, Mongkol; Sahasithiwat, Somboon; Zenno, Hikaru; Hayami, Shinya; Azam, Mohammad; Al-Resayes, Saud I; Chainok, Kittipong; Dalton Transactions  (2022) –; doi:10.1039/D2DT00007E

data_7710032
_publ_section_title
;
 Four series of lanthanide coordination polymers based on the
 tetrabromobenzene-1,4-dicarboxylate ligand: structural diversity and
 multifunctional properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00007E
_journal_year                    2022
_chemical_formula_moiety
'C20 H44.04 Br4 O20.04 Tb2, 2(Br4 C8 O4), 4(H2 O)'
_chemical_formula_sum            'C36 H52.04 Br12 O32.04 Tb2'
_chemical_formula_weight         2274.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-12-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                78.8140(10)
_cell_angle_beta                 82.6170(10)
_cell_angle_gamma                82.6250(10)
_cell_formula_units_Z            1
_cell_length_a                   10.4965(3)
_cell_length_b                   12.3708(3)
_cell_length_c                   12.7873(3)
_cell_measurement_reflns_used    9820
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      31.39
_cell_measurement_theta_min      3.13
_cell_volume                     1606.23(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            68573
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.506
_diffrn_reflns_theta_min         3.128
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.730
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5698
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0976 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.7635.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.351
_exptl_crystal_description       plate
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.00151(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         10691
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+1.7549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9004
_reflns_number_total             10691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00007e2.cif
_cod_data_source_block           3tb'
_cod_database_code               7710032
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.593
_shelx_estimated_absorpt_t_min   0.273
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 O5-H5
 0.85 with sigma of 0.01
 O6-H6
 0.85 with sigma of 0.01
 O7B-H7B
 0.85 with sigma of 0.01
 O4-H4
 0.82 with sigma of 0.02
 O7A-H7A
 0.85 with sigma of 0.01
 C5-H3
 1.893693 with sigma of 0.02
 Tb1-H3
 3.073972 with sigma of 0.02
 C7-H5
 1.894238 with sigma of 0.02
 Tb1-H5
 3.078564 with sigma of 0.02
 C8-H6
 1.900962 with sigma of 0.02
 Tb1-H6
 3.051202 with sigma of 0.02
 C9B-H7B
 1.906142 with sigma of 0.02
 Tb1-H7B
 2.790684 with sigma of 0.02
 C9A-H7A
 1.888504 with sigma of 0.02
 Tb1-H7A
 2.922925 with sigma of 0.02
 O7A-C9A \\sim O7B-C9B \\sim O8A-C10A \\sim O8B-C10B
 with sigma of 0.02
 C9A-C10A \\sim C9B-C10B
 with sigma of 0.02
 O4-C6B \\sim O3-C5
 with sigma of 0.02
 O4-C6A \\sim O3-C5
 with sigma of 0.02
 C6B-C5 \\sim C6A-C5
 with sigma of 0.02
 O4-C6B \\sim C5-O3
 with sigma of 0.02
 O4-C6A \\sim C5-O3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O7A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(O8A)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(O8B) \\sim Ueq, Uanis(C10B) \\sim Ueq, Uanis(C9B) \\sim Ueq, Uanis(O7B)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O7A, O8A, C9A, C10A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O7B, O8B, C9B, C10B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O3, O4, C5, C6B
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O3, O4, C5, C6A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Fixed Sof: O7A(0.02) H7A(0.02) O8A(0.2) H8A(0.2) O8B(0.8) H8B(0.8) C6A(0.75)
 H6AA(0.75) H6AB(0.75) C6B(0.25) H6BA(0.25) H6BB(0.25) C9A(0.2) H9AA(0.2)
 H9AB(0.2) C9B(0.8) H9BA(0.8) H9BB(0.8) C10A(0.2) H10C(0.2) H10D(0.2) C10B(0.8)
 H10E(0.8) H10F(0.8)
6.a Free rotating group:
 O15(H15A,H15B), O16(H16A,H16B)
6.b Rotating group:
 O9(H9A,H9B), O10(H10A,H10B)
6.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C7(H7C,H7D), C8(H8C,H8D),
 C9A(H9AA,H9AB), C9B(H9BA,H9BB), C10A(H10C,H10D), C10B(H10E,H10F)
6.d Idealised tetrahedral OH refined as rotating group:
 O8A(H8A), O8B(H8B)
;
_shelx_res_checksum              82857
_olex2_submission_special_instructions 'No special instructions were received'