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_7710021
_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         'C26.7 H15.4 Br12 Gd2 O17'
_chemical_formula_sum            'C26.7 H15.4 Br12 Gd2 O17'
_chemical_formula_weight         1881.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-12 deposited with the CCDC.	2022-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.686(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.587(5)
_cell_length_b                   18.133(7)
_cell_length_c                   21.632(9)
_cell_measurement_reflns_used    9627
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.025
_cell_measurement_theta_min      2.941
_cell_volume                     4504(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'PHOTON 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 D8 QUEST CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  'graphiteDouble Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64054
_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         25.999
_diffrn_reflns_theta_min         2.863
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\mus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.629
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1220 before and 0.0701 after correction. The Ratio of minimum to maximum transmission is 0.8762. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.775
_exptl_crystal_description       plate
_exptl_crystal_F_000             3438
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       0.00025(2)
_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   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         8850
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0326
_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/[\s^2^(Fo^2^)+(0.0202P)^2^+15.1813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6542
_reflns_number_total             8850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00007e2.cif
_cod_data_source_block           13gd
_cod_original_formula_sum        'C26.70 H15.40 Br12 Gd2 O17'
_cod_database_code               7710021
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.343
_shelx_estimated_absorpt_t_min   0.171
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O14-H14
 0.85 with sigma of 0.01
 O17-H17
 0.85 with sigma of 0.01
 O13A-H13A
 0.85 with sigma of 0.01
 O13-H13
 0.85 with sigma of 0.01
 O15-H15A = O15-H15B
 0.85 with sigma of 0.02
 O16-H16A = O16-H16B
 0.85 with sigma of 0.02
 C26-H14
 1.915338 with sigma of 0.02
 Gd2-H14
 2.96379 with sigma of 0.02
 C27-H17
 1.91147 with sigma of 0.02
 Gd2-H17
 3.083201 with sigma of 0.02
 C25A-H13A
 2.001639 with sigma of 0.02
 Gd2-H13A
 2.970671 with sigma of 0.02
 C25-H13
 2.006304 with sigma of 0.02
 Gd2-H13
 2.996201 with sigma of 0.02
 H15A-H15B
 1.34 with sigma of 0.04
 H16A-H16B
 1.34 with sigma of 0.04
 Gd2-O15 \\sim Gd2-O18
 with sigma of 0.01
 Gd2-O14 \\sim Gd2-O17
 with sigma of 0.01
 O14-C26 \\sim O17-C27
 with sigma of 0.01
 Gd2-O13 \\sim Gd2-O13A
 with sigma of 0.02
 O13-C25 \\sim O13A-C25A
 with sigma of 0.02
 Gd2-C25 \\sim Gd2-C25A
 with sigma of 0.04
 Gd2-H15A \\sim Gd2-H15B
 with sigma of 0.02
 Gd2-H16A \\sim Gd2-H16B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O17) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O13A) \\sim Ueq, Uanis(C25A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Gd2, O17, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Gd2, O18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Gd2, O13, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Gd2, O13A, C25A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O13A)=Sof(H13A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(O13)=Sof(H13)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Fixed Sof: O17(0.7) H17(0.7) O18(0.3) H18A(0.3) H18B(0.3) C27(0.7) H27A(0.7)
 H27B(0.7) H27C(0.7)
6.a Rotating group:
 O18(H18A,H18B)
6.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              12633
_olex2_submission_special_instructions 'No special instructions were received'