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_7130722
_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 O16 Y2, 2(C5.25 H11.25 N)'
_chemical_formula_sum            'C42.5 H38.5 N2 O16 Y2'
_chemical_formula_weight         1011.07
_chemical_name_systematic        KGF-15(Y)
_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
_atom_sites_solution_primary     dual
_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                   17.0356(5)
_cell_length_b                   47.4052(16)
_cell_length_c                   11.4193(4)
_cell_measurement_reflns_used    9448
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.1830
_cell_measurement_theta_min      1.7180
_cell_volume                     9222.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00  70.00   0.50    9.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    9.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0024120000
_diffrn_orient_matrix_UB_12      0.0230040000
_diffrn_orient_matrix_UB_13      0.0124632000
_diffrn_orient_matrix_UB_21      -0.0029220000
_diffrn_orient_matrix_UB_22      0.0346168000
_diffrn_orient_matrix_UB_23      -0.0082816000
_diffrn_orient_matrix_UB_31      -0.0619884000
_diffrn_orient_matrix_UB_32      -0.0025054000
_diffrn_orient_matrix_UB_33      -0.0000978000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37729
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.718
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             4108
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Flack x determined using 1652 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         10550
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1578
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0677P)^2^+21.4697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4980
_reflns_number_total             10550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04985f3.cif
_cod_data_source_block           yu350_8
_cod_original_formula_sum        'C42.50 H38.50 N2 O16 Y2'
_cod_database_code               7130722
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.950
_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(C21) = Uanis(N2) = Uanis(C27) = Uanis(C35) = Uanis(C37) = Uanis(C38) =
Uanis(C42) = Uanis(C43)
Uanis(N1) = Uanis(C26) = Uanis(C29) = Uanis(C32) = Uanis(C34) = Uanis(C36) =
Uanis(C40) = Uanis(C41)
Uanis(O1) = Uanis(O4) = Uanis(O6) = Uanis(O9) = Uanis(C2) = Uanis(C4) =
Uanis(C8) = Uanis(C10) = Uanis(C17) = Uanis(C18) = Uanis(C20) = Uanis(C30)
Uanis(O2) = Uanis(O3) = Uanis(O7) = Uanis(C1) = Uanis(O11) = Uanis(C3) =
Uanis(C6) = Uanis(C7) = Uanis(C9) = Uanis(C12) = Uanis(C19) = Uanis(C23)
Uanis(O13) = Uanis(C39) = Uanis(O16) = Uanis(C44) = Uanis(C46) = Uanis(C45)
Uanis(O5) = Uanis(C15) = Uanis(O12) = Uanis(C5) = Uanis(C25) = Uanis(C31)
Uanis(O8) = Uanis(O10) = Uanis(O14) = Uanis(C11) = Uanis(C13) = Uanis(O15) =
Uanis(C14) = Uanis(C16) = Uanis(C22) = Uanis(C24) = Uanis(C28) = Uanis(C33)
3. Others
 Fixed Sof: C21(0.75) H21A(0.75) H21B(0.75) H21C(0.75) C26(0.75) C27(0.75)
 H27A(0.75) H27B(0.75) C29(0.75) H29A(0.75) H29B(0.75) C32(0.75) H32A(0.75)
 H32B(0.75) H32C(0.75) C34(0.75) H34A(0.75) H34B(0.75) H34C(0.75) C35(0.75)
 C36(0.75) H36A(0.75) H36B(0.75) C37(0.75) H37A(0.75) H37B(0.75) H37C(0.75)
 C38(0.75) H38A(0.75) H38B(0.75) H38C(0.75) C40(0.75) H40A(0.75) H40B(0.75)
 C41(0.75) H41A(0.75) H41B(0.75) H41C(0.75) C42(0.75) H42A(0.75) H42B(0.75)
 C43(0.75) H43A(0.75) H43B(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C29(H29A,H29B), C36(H36A,H36B), C40(H40A,H40B), C42(H42A,
 H42B), C43(H43A,H43B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C11(H11), C16(H16), C17(H17), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25), C30(H30), C31(H31), C45(H45), C46(H46)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              27158
_shelx_hkl_checksum              38261
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.382
_oxdiff_exptl_absorpt_empirical_full_min 0.738