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_7130720
_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_formula_moiety         'C32 H16 Gd2 O16, 2(C5.25 H11.25 N)'
_chemical_formula_sum            'C42.5 H38.5 Gd2 N2 O16'
_chemical_formula_weight         1147.75
_chemical_name_systematic        KGF-15(Gd)
_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             2022-04-28
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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                   47.5920(11)
_cell_length_b                   17.2469(4)
_cell_length_c                   11.4052(2)
_cell_measurement_reflns_used    10254
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.2170
_cell_measurement_theta_min      2.3540
_cell_volume                     9361.6(3)
_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      150
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            22021
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.696
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.444
_exptl_absorpt_coefficient_mu    2.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77548
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       plate
_exptl_crystal_F_000             4508
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.29(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         7489
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+10.8213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.345
_reflns_Friedel_fraction_full    0.411
_reflns_Friedel_fraction_max     0.376
_reflns_number_gt                5407
_reflns_number_total             7489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04985f3.cif
_cod_data_source_block           ydkr_a_CCDC1
_cod_original_formula_sum        'C42.50 H38.50 Gd2 N2 O16'
_cod_database_code               7130720
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.762
_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. Others
 Fixed Sof: C8(0.75) H8A(0.75) H8B(0.75) H8C(0.75) C10(0.75) H10A(0.75)
 H10B(0.75) H10C(0.75) C23(0.75) H23A(0.75) H23B(0.75) H23C(0.75) C25(0.75)
 C26(0.75) H26A(0.75) H26B(0.75) C30(0.75) H30A(0.75) H30B(0.75) C31(0.75)
 H31A(0.75) H31B(0.75) C35(0.75) H35A(0.75) H35B(0.75) C36(0.75) H36A(0.75)
 H36B(0.75) H36C(0.75) C38(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) H43C(0.75)
 C45(0.75) H45A(0.75) H45B(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C30(H30A,H30B), C31(H31A,H31B), C35(H35A,H35B), C39(H39A,
 H39B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C9(H9), C12(H12), C13(H13), C18(H18), C19(H19),
 C20(H20), C22(H22), C24(H24), C32(H32), C33(H33), C34(H34), C42(H42), C44(H44)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C23(H23A,H23B,H23C), C36(H36A,H36B,
 H36C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              83896
_shelx_hkl_checksum              41423
_olex2_submission_special_instructions 'No special instructions were received'