Extended isomerism in heteronuclear metal–organic frameworks: synthetic strategies and crystal structures of lanthanide–cobalt–oxydiacetate systems
Igoa Saldaña, Fernando; López, Agustín; González-Platas, Javier; Suescun, Leopoldo; Kremer, Carlos; Torres, Julia; CrystEngComm 26 (2024) 2560–2570; doi:10.1039/D4CE00168K

data_7248412
_publ_section_title
;
 Extended isomerism in heteronuclear metal--organic frameworks: synthetic
 strategies and crystal structures of lanthanide--cobalt--oxydiacetate
 systems
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              2560
_journal_page_last               2570
_journal_paper_doi               10.1039/D4CE00168K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C24 H24 Co2 O30 Tb2, Co H12 O6, 3(O)'
_chemical_formula_sum            'C24 H36 Co3 O39 Tb2'
_chemical_formula_weight         1443.16
_space_group_crystal_system      cubic
_space_group_IT_number           228
_space_group_name_Hall           '-F 4ud 2vw 3'
_space_group_name_H-M_alt        'F d -3 c :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-28 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   25.6646(11)
_cell_length_b                   25.6646(11)
_cell_length_c                   25.6646(11)
_cell_measurement_reflns_used    2105
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.4190
_cell_measurement_theta_min      2.2310
_cell_volume                     16904.5(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -2.00  25.00   1.00    7.50    --   -0.39 -57.00-180.00   27
  2  \w    -70.00 -43.00   1.00    7.50    --   -0.39 -57.00-180.00   27
  3  \w     30.00  81.00   1.00   30.00    --   30.29  57.00 -30.00   51
  4  \w     58.00 112.00   1.00   30.00    --   30.29 178.00 -60.00   54
  5  \w    -37.00  48.00   1.00   30.00    --  -31.07  37.00 120.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0028669000
_diffrn_orient_matrix_UB_12      0.0214956000
_diffrn_orient_matrix_UB_13      -0.0170571000
_diffrn_orient_matrix_UB_21      0.0045641000
_diffrn_orient_matrix_UB_22      -0.0173522000
_diffrn_orient_matrix_UB_23      -0.0210797000
_diffrn_orient_matrix_UB_31      -0.0271165000
_diffrn_orient_matrix_UB_32      -0.0007616000
_diffrn_orient_matrix_UB_33      -0.0052787000
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            11380
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.243
_diffrn_reflns_theta_min         2.244
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.581
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_description       block
_exptl_crystal_F_000             11248
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.197
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+176.0718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                641
_reflns_number_total             881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00168k2.cif
_cod_data_source_block           cub_tbcooda
_cod_depositor_comments
'Adding full bibliography for 7248398--7248415.cif.'
_cod_original_cell_volume        16905(2)
_cod_original_sg_symbol_Hall     '-F 4cvw 2vw 3'
_cod_original_sg_symbol_H-M      'F d -3 c'
_cod_database_code               7248412
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C24 H36 Co3 Tb2 O39'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: O2W(0.25)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_shelx_res_checksum              90569
_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 2.484
_oxdiff_exptl_absorpt_empirical_full_min 0.855