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_7130724
_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 Er2 O16, 2(C5.25 H11.25 N)'
_chemical_formula_sum            'C42.5 H38.5 Er2 N2 O16'
_chemical_formula_weight         1167.77
_chemical_name_systematic        KGF-15(Er)
_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                   47.3291(14)
_cell_length_b                   16.9949(5)
_cell_length_c                   11.4233(3)
_cell_measurement_reflns_used    9414
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.0340
_cell_measurement_theta_min      2.2930
_cell_volume                     9188.4(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0906
_diffrn_reflns_av_unetI/netI     0.1038
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37542
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.721
_exptl_absorpt_coefficient_mu    3.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65057
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       plate
_exptl_crystal_F_000             4572
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Flack x determined using 1331 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.54(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         10443
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+59.4982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                4215
_reflns_number_total             10443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04985f3.cif
_cod_data_source_block           ydkr_a_CCDC3
_cod_original_formula_sum        'C42.50 H38.50 Er2 N2 O16'
_cod_database_code               7130724
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.947
_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(N2) = Uanis(C29) = Uanis(C31) = Uanis(C33) = Uanis(C34) = Uanis(C36) =
Uanis(C38) = Uanis(C41)
Uanis(N1) = Uanis(C30) = Uanis(C32) = Uanis(C35) = Uanis(C37) = Uanis(C39) =
Uanis(C45) = Uanis(C46)
Uanis(O1) = Uanis(C3) = Uanis(C4) = Uanis(O8) = Uanis(C16) = Uanis(C23) =
Uanis(C24) = Uanis(C26) = Uanis(C27) = Uanis(O15) = Uanis(C40) = Uanis(O16)
Uanis(O9) = Uanis(C15) = Uanis(C19) = Uanis(C21) = Uanis(C22) = Uanis(O10) =
Uanis(C25) = Uanis(O11) = Uanis(O12) = Uanis(C28) = Uanis(C43) = Uanis(C44)
Uanis(O2) = Uanis(O3) = Uanis(C7) = Uanis(C8) = Uanis(C11) = Uanis(C12) =
Uanis(C13) = Uanis(C14) = Uanis(C18) = Uanis(O13) = Uanis(O14) = Uanis(C42)
Uanis(C1) = Uanis(C2) = Uanis(O6) = Uanis(O7) = Uanis(C6) = Uanis(C9)
Uanis(O4) = Uanis(O5) = Uanis(C5) = Uanis(C10) = Uanis(C17) = Uanis(C20)
3. Others
 Fixed Sof: C29(0.75) C30(0.75) C31(0.75) H31A(0.75) H31B(0.75) H31C(0.75)
 C32(0.75) H32A(0.75) H32B(0.75) H32C(0.75) C33(0.75) H33A(0.75) H33B(0.75)
 C34(0.75) H34A(0.75) H34B(0.75) H34C(0.75) C35(0.75) H35A(0.75) H35B(0.75)
 C36(0.75) H36A(0.75) H36B(0.75) H36C(0.75) C37(0.75) H37A(0.75) H37B(0.75)
 C38(0.75) H38A(0.75) H38B(0.75) C39(0.75) H39A(0.75) H39B(0.75) H39C(0.75)
 C41(0.75) H41A(0.75) H41B(0.75) C45(0.75) H45A(0.75) H45B(0.75) C46(0.75)
 H46A(0.75) H46B(0.75) H46C(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C41(H41A,
 H41B), C45(H45A,H45B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C11(H11), C13(H13), C14(H14), C17(H17),
 C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C44(H44)
4.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              71092
_shelx_hkl_checksum              36535
_olex2_submission_special_instructions 'No special instructions were received'