Heterometallic palladium-iron metal-organic framework as a highly active catalyst for cross-coupling reactions.
Miguel-Casañ, Eugenia; Darawsheh, Mohanad D.; Fariña-Torres, Víctor; Vitórica-Yrezábal, Iñigo J; Andres-Garcia, Eduardo; Fañanás-Mastral, Martín; Mínguez Espallargas, Guillermo; Chemical science 14 (2022) 179–185; doi:10.1039/d2sc05192c

data_1567996
_publ_section_title
;
 Heterometallic palladium-iron metal-organic framework as a highly active
 catalyst for cross-coupling reactions.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              179
_journal_page_last               185
_journal_paper_doi               10.1039/d2sc05192c
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C42 H30 Cl6 Fe6 N6 O32 Pd3, 6(H2 O)'
_chemical_formula_sum            'C42 H42 Cl6 Fe6 N6 O38 Pd3'
_chemical_formula_weight         2105.81
_space_group_crystal_system      cubic
_space_group_IT_number           223
_space_group_name_Hall           '-P 4n 2 3'
_space_group_name_H-M_alt        'P m -3 n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-02-14 deposited with the CCDC.	2022-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1165(4)
_cell_length_b                   22.1165(4)
_cell_length_c                   22.1165(4)
_cell_measurement_reflns_used    1855
_cell_measurement_temperature    119.6(8)
_cell_measurement_theta_max      15.7940
_cell_measurement_theta_min      3.6700
_cell_volume                     10818.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.6(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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    -14.00  23.00   1.00   40.00    --  -14.89 -99.00 150.00   37
  2  \w    -84.00   7.00   1.00   40.00    --  -14.89 -57.00   0.00   91
  3  \w    -59.00  45.00   1.00   40.00    --  -14.89  19.00  90.00  104
  4  \w    -74.00 -38.00   1.00   40.00    --  -14.89 127.00 -22.20   36
  5  \w    -79.00   7.00   1.00   40.00    --  -14.89 -57.00-120.00   86
  6  \w      8.00  76.00   1.00   40.00    --   15.67-129.00 -35.56   68
  7  \w    -53.00  32.00   1.00   40.00    --   15.67 -57.00-120.00   85
  8  \w    -10.00  88.00   1.00   40.00    --   15.67  38.00-180.00   98
  9  \w    -54.00  46.00   1.00   40.00    --   15.67 -77.00 150.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0291090000
_diffrn_orient_matrix_UB_12      0.0041425000
_diffrn_orient_matrix_UB_13      0.0128225000
_diffrn_orient_matrix_UB_21      0.0134653000
_diffrn_orient_matrix_UB_22      -0.0079250000
_diffrn_orient_matrix_UB_23      -0.0280029000
_diffrn_orient_matrix_UB_31      -0.0004456000
_diffrn_orient_matrix_UB_32      0.0307997000
_diffrn_orient_matrix_UB_33      -0.0089246000
_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  0.2715
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54934
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        16.515
_diffrn_reflns_theta_max         16.515
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.070
_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     68
_refine_ls_number_reflns         544
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0831P)^2^+46.9800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                435
_reflns_number_total             544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05192c2.cif
_cod_data_source_block           muv22
_cod_depositor_comments
;Adding full bibliography for 1567996.cif.

 Adding full bibliography for 1567996.cif.
;
_cod_original_cell_volume        10818.1(6)
_cod_database_code               1567996
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Fe1-H4A \\sim Fe1-H4B
 with sigma of 0.02
3. Others
 Fixed Sof: H4A(0.5) H4B(0.5) Cl2(0.25) Cl1(0.25)
4.a Riding coordinates:
 O4(H4A,H4B), O5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9284
_shelx_fab_checksum              45271
_olex2_date_sample_data_collection 2019-02-20
_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 1.476
_oxdiff_exptl_absorpt_empirical_full_min 0.565