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_7248415
_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 H30 Co3 Gd2 O36, 1(O)'
_chemical_formula_sum            'C24 H30 Co3 Gd2 O37'
_chemical_formula_weight         1401.77
_space_group_crystal_system      hexagonal
_space_group_IT_number           192
_space_group_name_Hall           '-P 6 2c'
_space_group_name_H-M_alt        'P 6/m c c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-26
_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                120
_cell_formula_units_Z            2
_cell_length_a                   14.7363(5)
_cell_length_b                   14.7363(5)
_cell_length_c                   15.6706(6)
_cell_measurement_reflns_used    1935
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6040
_cell_measurement_theta_min      2.5990
_cell_volume                     2947.09(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(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 0.942
_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    -23.00  41.00   1.00   30.00    --  -26.73  57.00  30.00   64
  2  \w    -93.00 -45.00   1.00   30.00    --  -26.73-178.00  30.00   48
  3  \w     -1.00  52.00   1.00   30.00    --  -26.73  37.00 -90.00   53
;
_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      -0.0359476000
_diffrn_orient_matrix_UB_12      0.0115009000
_diffrn_orient_matrix_UB_13      -0.0205741000
_diffrn_orient_matrix_UB_21      -0.0068145000
_diffrn_orient_matrix_UB_22      -0.0357713000
_diffrn_orient_matrix_UB_23      -0.0330435000
_diffrn_orient_matrix_UB_31      -0.0418467000
_diffrn_orient_matrix_UB_32      -0.0409595000
_diffrn_orient_matrix_UB_33      0.0230714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6943
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.354
_diffrn_reflns_theta_min         1.596
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.130
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
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_density_diffrn    1.580
_exptl_crystal_F_000             1358
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0771P)^2^+11.9038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                888
_reflns_number_total             1212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00168k2.cif
_cod_data_source_block           gdco_1
_cod_depositor_comments
'Adding full bibliography for 7248398--7248415.cif.'
_cod_original_cell_volume        2947.1(2)
_cod_database_code               7248415
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C24 H50 O46 Co3 Gd'
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.546
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1W(0.5) O2W(0.08334)
3.a Rotating group:
 O1W(H1W)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_shelx_res_checksum              89593
_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 1.090
_oxdiff_exptl_absorpt_empirical_full_min 0.874