Structurally characterized dipalladium(ii)-oxamate metallacyclophanes as efficient catalysts for sustainable Heck and Suzuki reactions in ionic liquids
Fortea-Pérez, Francisco Ramón; El Idrissi Moubtassim, Mouly Lahcen; Armentano, Donatella; De Munno, Giovanni; Julve, Miguel; Stiriba, Salah-Eddine; Inorganic Chemistry Frontiers 5 (2018) 2148–; doi:10.1039/C8QI00498F

data_4349869
_publ_section_title
;
 Structurally characterized dipalladium(ii)-oxamate metallacyclophanes as
 efficient catalysts for sustainable Heck and Suzuki reactions in ionic
 liquids
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2148
_journal_paper_doi               10.1039/C8QI00498F
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C108 H192 N8 O20 Pd2'
_chemical_formula_weight         2135.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-05-28 deposited with the CCDC.
2018-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                102.903(2)
_cell_angle_beta                 102.983(2)
_cell_angle_gamma                105.397(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4534(7)
_cell_length_b                   14.7803(10)
_cell_length_c                   20.3003(13)
_cell_measurement_reflns_used    8721
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      2.4
_cell_volume                     2809.8(3)
_computing_cell_refinement       'Bruker APEX'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37656
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.151
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         9868
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+1.7150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9054
_reflns_number_total             9868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00498f2.cif
_cod_data_source_block           DATA4a
_cod_database_code               4349869
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.962
_shelxl_version_number           2013-4
_shelx_res_checksum              38288
_shelx_hkl_checksum              48898