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_7710025
_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         'C32 H32 Br12 O24 Tb2, 2(C2 H6 O2), 2(H2 O)'
_chemical_formula_sum            'C36 H48 Br12 O30 Tb2'
_chemical_formula_weight         2237.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-22 deposited with the CCDC.	2022-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.9410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.62280(10)
_cell_length_b                   22.3036(4)
_cell_length_c                   16.5045(3)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.297
_cell_measurement_theta_min      2.644
_cell_volume                     3157.09(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_detector                 'Bruker PHOTON 200 area detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 QUEST CMOS PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            63712
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.644
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_type              Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.896
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1127 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.7681.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.354
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.433
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         7834
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+5.9439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6927
_reflns_number_total             7834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00007e2.cif
_cod_data_source_block           3tb_r
_cod_database_code               7710025
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.338
_shelx_estimated_absorpt_t_min   0.200
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O12-H12B = O12-H12A = O15-H15E = O15-H15F
 0.84 with sigma of 0.01
 O7-C13A \\sim O7-C13B \\sim O8-C14A \\sim O8-C14A
 with sigma of 0.02
 C14A-C13B \\sim C14A-C13A
 with sigma of 0.02
 O7-C14A \\sim O8-C13A
 with sigma of 0.02
 O7-C14B \\sim O8-C13B
 with sigma of 0.02
 C18B-C17 \\sim C18A-C17
 with sigma of 0.02
 O14A-C18A \\sim O14B-C18B
 with sigma of 0.02
 O14A-C17 \\sim O14B-C17
 with sigma of 0.02
 O13-C18A \\sim O13-C18B
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 O10-C16 \\sim O10-C16A
 with sigma of 0.02
 O9-C15 \\sim O9-C15A
 with sigma of 0.02
 O9-C16 \\sim O9-C16A
 with sigma of 0.04
 O10-C15 \\sim O10-C15A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C14B) \\sim Ueq,
Uanis(O8) \\sim Ueq, Uanis(O14B) \\sim Ueq, Uanis(C18B) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14A) \\sim Ueq, Uanis(C18A) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O7, C13A, C14A, O8, O7, C13B, C14B, O8, O14B, C18B, C17, O13, O14A, C18A, C17,
  O13, O10, C16, C15, O9, O10, C16A, C15A, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H7B)=Sof(H8B)=Sof(C13B)=Sof(H13A)=Sof(H13B)=Sof(C14B)=Sof(H14C)=Sof(H14D)=
 1-FVAR(1)
 Sof(H7A)=Sof(H8A)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C13A)=Sof(H13C)=Sof(H13D)=
 FVAR(1)
 Sof(O14B)=Sof(H14E)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18C)=Sof(H18D)=1-FVAR(2)
 Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(O14A)=Sof(H14F)=FVAR(2)
 Sof(H9B)=Sof(H10A)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C15A)=Sof(H15C)=
 Sof(H15D)=1-FVAR(3)
 Sof(H9A)=Sof(H10)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 FVAR(3)
6.a Rotating group:
 O11(H11A,H11B), O12(H12A,H12B)
6.b Secondary CH2 refined with riding coordinates:
 C13B(H13A,H13B), C14A(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C17(H17C,H17D), C18A(H18A,H18B), C13A(H13C,H13D), C14B(H14C,H14D),
 C18B(H18C,H18D), C16A(H16C,H16D), C15A(H15C,H15D)
6.c Tetrahedral OH refined with riding coordinates:
 O7(H7B), O7(H7A), O8(H8A), O8(H8B), O9(H9A), O9(H9B), O10(H10), O10(H10A)
6.d Idealised tetrahedral OH refined as rotating group:
 O13(H13), O14B(H14E), O14A(H14F)
;
_shelx_res_checksum              8012
_olex2_submission_special_instructions 'No special instructions were received'