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_7240771
_publ_section_title
;
 Self-assembly of three-dimensional oxalate-bridged
 alkali(I)-lanthanide(III) heterometal-organic frameworks
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00099J
_journal_year                    2020
_chemical_formula_moiety         'C10.25 H4 Dy4 Na2 O25, 2.5(O)'
_chemical_formula_sum            'C10.25 H4 Dy4 Na2 O27.5'
_chemical_formula_weight         1263.11
_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
_atom_sites_solution_primary     dual
_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
;
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                   12.5277(3)
_cell_length_b                   12.5277(3)
_cell_length_c                   19.1754(8)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      3.13
_cell_volume                     3009.45(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0479
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13464
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.378
_diffrn_reflns_theta_min         3.131
_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    9.948
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0997 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.7306.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.788
_exptl_crystal_description       block
_exptl_crystal_F_000             2286
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.663
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1602
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0387P)^2^+56.7143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1377
_reflns_number_total             1602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00099j2.cif
_cod_data_source_block           2dy
_cod_original_cell_volume        3009.45(19)
_cod_original_formula_sum        'C10.25 H4 Dy4 Na2 O27.50'
_cod_database_code               7240771
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.199
_shelx_estimated_absorpt_t_min   0.167
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.478(2)
 0.522(2)
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.001
 Dy1_$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(Dy1) \\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)
;
_shelx_res_checksum              53484
_olex2_submission_special_instructions 'No special instructions were received'