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_7240769
_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         'C21 H15 Er8 Na4 O50, 9.6[H2O]'
_chemical_formula_sum            'C21 H15 Er8 Na4 O50'
_chemical_formula_weight         2497.37
_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             2019-10-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_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            2
_cell_length_a                   12.4441(2)
_cell_length_b                   12.4441(2)
_cell_length_c                   19.0521(5)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    296.0
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      3.15
_cell_volume                     2950.32(10)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'XT n/a (Sheldrick, 2015)'
_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 0.998
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 QUEST CMOS PHOTON II'
_diffrn_measurement_method       '\w and \f 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  0.0287
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20538
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         3.152
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Micro focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.385
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0638 before and 0.0410 after correction.
The Ratio of minimum to maximum transmission is 0.8263.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.811
_exptl_crystal_description       block
_exptl_crystal_F_000             2258
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.802
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1891
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0050P)^2^+37.7606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1706
_reflns_number_total             1891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00099j2.cif
_cod_data_source_block           3er
_cod_original_cell_volume        2950.32(13)
_cod_database_code               7240769
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.299
_shelx_estimated_absorpt_t_min   0.234
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 Na1, O7, C4
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Fixed Sof: O3A(0.5) O3B(0.5) O4A(0.5) O4B(0.5) O5A(0.5) O5B(0.5) O6A(0.5)
 O6B(0.5) O7(0.25) H7(0.125) C3A(0.5) C3B(0.5) C4(0.125) H4C(0.25) H4A(0.25)
 H4B(0.25)
 Fixed X: O7(0.436688) C4(0.5)
 Fixed Y: O7(0.563621) C4(0.5)
 Fixed Z: O7(0.5) C4(0.534289)
6.a Riding coordinates:
 O7(H7), C4(H4C,H4A,H4B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64783
_shelx_fab_checksum              77901
_olex2_submission_special_instructions 'No special instructions were received'