Temperature-dependent 3D structures of lanthanide coordination polymers based on dicarboxylate mixed ligands
Chainok, Kittipong; Ponjan, Nutcha; Theppitak, Chatphorn; Khemthong, Phailyn; Kielar, Filip; Dungkaew, Winya; Zhou, Yan; Batten, Stuart R.; CrystEngComm 20 (2018) 7446–; doi:10.1039/C8CE01430B

data_7231580
_publ_section_title
;
 Temperature-dependent 3D structures of lanthanide coordination polymers
 based on dicarboxylate mixed ligands
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              7446
_journal_paper_doi               10.1039/C8CE01430B
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H16 O16 Tb2, 2(H2 O)'
_chemical_formula_sum            'C16 H20 O18 Tb2'
_chemical_formula_weight         818.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-08-24 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1226(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9635(3)
_cell_length_b                   12.4252(4)
_cell_length_c                   10.3811(4)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.197
_cell_measurement_theta_min      3.171
_cell_volume                     1125.99(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 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      296.0
_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 0.995
_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  0.0684
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38307
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.380
_diffrn_reflns_theta_min         2.852
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Incoatec I\mus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.320
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0806 before and 0.0695 after correction. The Ratio of minimum to maximum transmission is 0.8828. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.413
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.009
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.451(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5578
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0508
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5030
_reflns_number_total             5578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01430b2.cif
_cod_data_source_block           5tb
_cod_depositor_comments
'Adding full bibliography for 7231570--7231583.cif.'
_cod_database_code               7231580
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.431
_shelx_estimated_absorpt_t_min   0.365
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.549(17)
 0.451(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 O14-H14A = O16-H16A
 0.84 with sigma of 0.01
 O14-H14B
 0.84 with sigma of 0.01
 H14A-H14B
 1.37 with sigma of 0.02
 O17-H17A
 0.84 with sigma of 0.01
 O16-H16B
 0.84 with sigma of 0.01
 H16A-H16B
 1.355 with sigma of 0.02
 O17-H17B
 0.84 with sigma of 0.01
 H17A-H17B
 1.365 with sigma of 0.02
 O13-H13A
 0.84 with sigma of 0.01
 O15-H15A
 0.84 with sigma of 0.01
 O15-H15B
 0.84 with sigma of 0.01
 H15B-H15A
 1.37 with sigma of 0.02
 O18-H18A
 0.84 with sigma of 0.01
 O18-H18B
 0.84 with sigma of 0.01
 H18A-H18B
 1.37 with sigma of 0.02
 O13-H13B
 0.84 with sigma of 0.01
 H13A-H13B
 1.355 with sigma of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C14(H14), C15(H15)
;
_shelx_res_checksum              20728
_olex2_submission_special_instructions 'No special instructions were received'