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_7130721
_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 Eu2 O16, 2(C5.25 H11.25 N)'
_chemical_formula_sum            'C42.5 H38.5 Eu2 N2 O16'
_chemical_formula_weight         1137.17
_chemical_name_systematic        KGF-15(Eu)
_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                   47.3677(3)
_cell_length_b                   17.29520(10)
_cell_length_c                   11.31890(10)
_cell_measurement_reflns_used    61004
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.719
_cell_measurement_theta_min      1.600
_cell_volume                     9272.83(11)
_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, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.780
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4131
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.780
_diffrn_reflns_limit_h_max       84
_diffrn_reflns_limit_h_min       -83
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            61004
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.757
_diffrn_reflns_theta_full        14.351
_diffrn_reflns_theta_max         21.719
_diffrn_reflns_theta_min         1.600
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48688
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             4492
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.811
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 6890 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         21130
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+11.5082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.733
_reflns_number_gt                17081
_reflns_number_total             21130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04985f3.cif
_cod_data_source_block           ydkr_a_CCDC2
_cod_original_formula_sum        'C42.50 H38.50 Eu2 N2 O16'
_cod_database_code               7130721
_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. Others
 Sof(C47)=Sof(H37b)=1-FVAR(1)
 Sof(C37)=Sof(H37a)=FVAR(1)
 Fixed Sof: C13(0.75) H13a(0.75) H13b(0.75) H13c(0.75) C23(0.75) H23a(0.75)
 H23b(0.75) C26(0.75) C31(0.75) H31a(0.75) H31b(0.75) C33(0.75) H33a(0.75)
 H33b(0.75) H33c(0.75) C35(0.75) H35a(0.75) H35b(0.75) C36(0.75) H36a(0.75)
 H36b(0.75) C39(0.75) H39a(0.75) H39b(0.75) H39c(0.75) C40(0.75) H40a(0.75)
 H40b(0.75) H40c(0.75) C42(0.75) H42a(0.75) H42b(0.75) H42c(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)
3.a Secondary CH2 refined with riding coordinates:
 C23(H23a,H23b), C31(H31a,H31b), C35(H35a,H35b), C36(H36a,H36b), C43(H43a,
 H43b), C44(H44a,H44b)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C10(H10), C12(H12), C16(H16), C20(H20), C21(H21), C22(H22),
 C25(H25), C29(H29), C30(H30), C32(H32), C34(H34), C37(H37a), C38(H38),
 C41(H41), C47(H37b)
3.c Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C33(H33a,H33b,H33c), C39(H39a,H39b,H39c), C40(H40a,H40b,
 H40c), C42(H42a,H42b,H42c), C46(H46a,H46b,H46c)
;
_shelx_res_checksum              88780
_shelx_hkl_checksum              18741
_olex2_submission_special_instructions 'No special instructions were received'