Self-assembly of three-dimensional oxalate-bridged alkali(I)-lanthanide(III) heterometal-organic frameworks
Ponjan, Nutcha; Kielar, Filip; Dungkaew, Winya; Kongpatpanich, Kanokwan; Zenno, Hikaru; Hayami, Shinya; Sukwattanasinitt, Mongkol; Chainok, Kittipong; CrystEngComm  (2020) –; doi:10.1039/D0CE00099J

data_7240770
_publ_section_title
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 Self-assembly of three-dimensional oxalate-bridged
 alkali(I)-lanthanide(III) heterometal-organic frameworks
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00099J
_journal_year                    2020
_chemical_formula_moiety         'C10.25 H4 Na2 O25 Tb4, 2.5(O)'
_chemical_formula_sum            'C10.25 H4 Na2 O27.5 Tb4'
_chemical_formula_weight         1248.79
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2020-01-08
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
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2020-01-07 deposited with the CCDC.	2020-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5792(4)
_cell_length_b                   12.5792(4)
_cell_length_c                   19.2471(8)
_cell_measurement_reflns_used    6455
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      25.981
_cell_measurement_theta_min      3.119
_cell_volume                     3045.59(19)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 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      296.0
_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 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  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  0.0693
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20225
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         3.239
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.305
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.2024 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.8224.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.724
_exptl_crystal_description       block
_exptl_crystal_F_000             2270
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.845
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1553
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0208P)^2^+184.9491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1355
_reflns_number_total             1553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00099j2.cif
_cod_data_source_block           1tb
_cod_original_cell_volume        3045.6(2)
_cod_original_formula_sum        'C10.25 H4 Na2 O27.50 Tb4'
_cod_database_code               7240770
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.214
_shelx_estimated_absorpt_t_min   0.180
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.499(4)
 0.501(4)
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.001
 Tb1_$2-H1
 2.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O6A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O3B) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(C3B)
\\sim Ueq, Uanis(O5B) \\sim Ueq, Uanis(O6B) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Tb1) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O3A, O4A, O5A, O6A, C2, C3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3B, O4B, O5B, O6B, C2, C3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O3(0.25) O3A(0.5) O3B(0.5) O4(0.5) O4A(0.5) O4B(0.5) O5(0.125)
 O5A(0.5) O5B(0.5) O6A(0.5) O6B(0.5) C1(0.0625) C3A(0.5) C3B(0.5)
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_shelx_res_checksum              41168
_olex2_submission_special_instructions 'No special instructions were received'