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_7130723
_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 Dy2 O16, 2(C5.25 H11.25 N)'
_chemical_formula_sum            'C42.5 H38.5 Dy2 N2 O16'
_chemical_formula_weight         1158.25
_chemical_name_systematic        KGF-15(Dy)
_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                   17.26240(10)
_cell_length_b                   47.8338(4)
_cell_length_c                   11.47730(10)
_cell_measurement_reflns_used    11437
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.3030
_cell_measurement_theta_min      1.7520
_cell_volume                     9477.11(13)
_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      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.752
_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      0.00 177.50   0.50    1.00    --    0.00  45.00   0.00  355
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0119197000
_diffrn_orient_matrix_UB_12      -0.0089778000
_diffrn_orient_matrix_UB_13      -0.0075867000
_diffrn_orient_matrix_UB_21      0.0012491000
_diffrn_orient_matrix_UB_22      -0.0221126000
_diffrn_orient_matrix_UB_23      0.0035240000
_diffrn_orient_matrix_UB_31      -0.0343458000
_diffrn_orient_matrix_UB_32      -0.0039263000
_diffrn_orient_matrix_UB_33      -0.0025111000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4176
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.752
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -68
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58647
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.726
_diffrn_reflns_theta_full        14.511
_diffrn_reflns_theta_max         21.613
_diffrn_reflns_theta_min         1.501
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72135
_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    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             4540
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.983
_refine_diff_density_min         -2.224
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details
;
 Flack x determined using 3873 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.43(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         19774
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+35.0308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1316
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.698
_reflns_number_gt                11045
_reflns_number_total             19774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04985f3.cif
_cod_data_source_block           yu347_33_
_cod_original_formula_sum        'C42.50 H38.50 Dy2 N2 O16'
_cod_database_code               7130723
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32O32Dy2
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.977
_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(C20) = Uanis(C45) = Uanis(C30) = Uanis(C40) = Uanis(C37) = Uanis(C43) =
Uanis(C44)
Uanis(C29) = Uanis(C24) = Uanis(C42) = Uanis(C26) = Uanis(C46) = Uanis(C31) =
Uanis(C38)
Uanis(O11) = Uanis(O3) = Uanis(C11) = Uanis(C6) = Uanis(C23) = Uanis(C12)
Uanis(C10) = Uanis(C18) = Uanis(C14) = Uanis(C21) = Uanis(C17) = Uanis(C33) =
Uanis(C19) = Uanis(C22)
Uanis(C2) = Uanis(C27) = Uanis(C28) = Uanis(C35)
Uanis(C8) = Uanis(C16) = Uanis(C32) = Uanis(C39) = Uanis(C13) = Uanis(C36) =
Uanis(C25) = Uanis(C34)
Uanis(C1) = Uanis(C9) = Uanis(C3) = Uanis(C15) = Uanis(C5) = Uanis(C41) =
Uanis(C7) = Uanis(C4)
3. Others
 Fixed Sof: C20(0.75) H20A(0.75) H20B(0.75) H20C(0.75) C24(0.75) H24A(0.75)
 H24B(0.75) C26(0.75) C29(0.75) H29A(0.75) H29B(0.75) H29C(0.75) C30(0.75)
 H30A(0.75) H30B(0.75) C31(0.75) H31A(0.75) H31B(0.75) H31C(0.75) C37(0.75)
 H37A(0.75) H37B(0.75) H37C(0.75) C38(0.75) H38A(0.75) H38B(0.75) C40(0.75)
 H40A(0.75) H40B(0.75) C42(0.75) H42A(0.75) H42B(0.75) C43(0.75) H43A(0.75)
 H43B(0.75) C44(0.75) H44A(0.75) H44B(0.75) H44C(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:
 C24(H24A,H24B), C30(H30A,H30B), C38(H38A,H38B), C40(H40A,H40B), C42(H42A,
 H42B), C43(H43A,H43B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C12(H12), C14(H14), C15(H15), C19(H19), C21(H21),
 C23(H23), C25(H25), C28(H28), C32(H32), C33(H33), C35(H35), C36(H36), C39(H39)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C37(H37A,H37B,
 H37C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              95905
_shelx_hkl_checksum              69166
_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 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.858