Data-driven efficient synthetic exploration of anionic lanthanide-based metal–organic frameworks
Kitamura, Yu; Nakamura, Yuiga; Sugimoto, Kunihisa; Yoshikawa, Hirofumi; Tanaka, Daisuke; Chemical Communications  (2022) –; doi:10.1039/D2CC04985F

data_7130726
_publ_section_title
;
 Data-driven efficient synthetic exploration of anionic lanthanide-based
 metal--organic frameworks
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04985F
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H16 O16 Tb2, 2(C5.25 H11.25 N)'
_chemical_formula_sum            'C42.5 H38.5 N2 O16 Tb2'
_chemical_formula_weight         1151.09
_chemical_name_systematic        KGF-15(Tb)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-04-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2022-05-02 deposited with the CCDC.	2022-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   47.3077(4)
_cell_length_b                   17.1468(2)
_cell_length_c                   11.34970(10)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.4670
_cell_measurement_theta_min      1.7120
_cell_volume                     9206.60(16)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.771
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4126
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.771
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            60936
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.741
_diffrn_reflns_theta_full        14.333
_diffrn_reflns_theta_max         21.793
_diffrn_reflns_theta_min         1.499
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65021
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       plate
_exptl_crystal_F_000             4524
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.974
_refine_diff_density_min         -2.780
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details
;
 Flack x determined using 4276 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.45(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         20830
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0285P)^2^+26.1049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.708
_reflns_number_gt                11870
_reflns_number_total             20830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04985f3.cif
_cod_data_source_block           ydkr_a_CCDC5
_cod_original_formula_sum        'C42.50 H38.50 N2 O16 Tb2'
_cod_database_code               7130726
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C8) = Uanis(C5) = Uanis(C2) = Uanis(C3) = Uanis(C31) =
Uanis(C14) = Uanis(C6)
Uanis(C12) = Uanis(C18) = Uanis(C21) = Uanis(C26) = Uanis(C24) = Uanis(C20) =
Uanis(C27) = Uanis(C22)
Uanis(C10) = Uanis(C16) = Uanis(C13) = Uanis(C38)
Uanis(C40) = Uanis(C35) = Uanis(C37) = Uanis(C42)
3. Others
 Fixed Sof: C4(0.75) H4A(0.75) H4B(0.75) H4C(0.75) C9(0.75) H9A(0.75)
 H9B(0.75) C11(0.75) H11A(0.75) H11B(0.75) C15(0.75) C29(0.75) H29A(0.75)
 H29B(0.75) H29C(0.75) C30(0.75) H30A(0.75) H30B(0.75) H30C(0.75) C32(0.75)
 H32A(0.75) H32B(0.75) C36(0.75) H36A(0.75) H36B(0.75) H36C(0.75) C39(0.75)
 H39A(0.75) H39B(0.75) C41(0.75) H41A(0.75) H41B(0.75) H41C(0.75) C43(0.75)
 H43A(0.75) H43B(0.75) C44(0.75) H44A(0.75) H44B(0.75) C45(0.75) C46(0.75)
 H46A(0.75) H46B(0.75) H46C(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C32(H32A,H32B), C39(H39A,H39B), C43(H43A,H43B),
 C44(H44A,H44B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C14(H14), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22),
 C25(H25), C26(H26), C28(H28), C31(H31), C33(H33), C35(H35), C38(H38), C42(H42)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C36(H36A,H36B,
 H36C), C41(H41A,H41B,H41C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              61856
_shelx_hkl_checksum              80005
_olex2_submission_special_instructions 'No special instructions were received'