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_7248405
_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 O36 Pr2, 4.5(O)'
_chemical_formula_sum            'C24 H30 Co3 O40.5 Pr2'
_chemical_formula_weight         1425.09
_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             2023-08-29
_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                120
_cell_formula_units_Z            2
_cell_length_a                   15.2346(3)
_cell_length_b                   15.2346(3)
_cell_length_c                   15.2447(3)
_cell_measurement_reflns_used    4358
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.6900
_cell_measurement_theta_min      2.6630
_cell_volume                     3064.16(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     -1.00  25.00   1.00    7.50    --   -0.39  77.00 150.00   26
  2  \w    -36.00  -6.00   1.00    7.50    --   -0.39  77.00 150.00   30
  3  \w     92.00 119.00   1.00   30.00    --   30.13 178.00-150.00   27
  4  \w     59.00 113.00   1.00   30.00    --   30.13 178.00 -90.00   54
  5  \w    -61.00  43.00   1.00   30.00    --  -30.91  57.00 120.00  104
;
_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      0.0425408000
_diffrn_orient_matrix_UB_12      0.0260330000
_diffrn_orient_matrix_UB_13      0.0280459000
_diffrn_orient_matrix_UB_21      -0.0053376000
_diffrn_orient_matrix_UB_22      -0.0469614000
_diffrn_orient_matrix_UB_23      0.0135533000
_diffrn_orient_matrix_UB_31      0.0324428000
_diffrn_orient_matrix_UB_32      0.0026783000
_diffrn_orient_matrix_UB_33      -0.0345531000
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9653
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.672
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.830
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             1394
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.365
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1330
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0394
_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^)+(0.0878P)^2^+4.9435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1089
_reflns_number_total             1330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00168k2.cif
_cod_data_source_block           hex_prcooda
_cod_depositor_comments
'Adding full bibliography for 7248398--7248415.cif.'
_cod_original_cell_volume        3064.17(13)
_cod_original_formula_sum        'C24 H30 Co3 O40.50 Pr2'
_cod_database_code               7248405
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         Pr2Co3C24H36O40
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.737
_reflns_odcompleteness_completeness 99.74
_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
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1W-H1W
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: H1W(0.5) O2W(0.125) O3W(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_shelx_res_checksum              78269
_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 1.253
_oxdiff_exptl_absorpt_empirical_full_min 0.810