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_4349868
_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            'C114 H208 N8 O20 Pd2'
_chemical_formula_weight         2223.67
_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                70.239(2)
_cell_angle_beta                 76.719(2)
_cell_angle_gamma                70.278(2)
_cell_formula_units_Z            1
_cell_length_a                   12.0326(5)
_cell_length_b                   14.1370(6)
_cell_length_c                   20.7121(9)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.2
_cell_measurement_theta_min      2.2
_cell_volume                     3094.5(2)
_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 0.650
_diffrn_measured_fraction_theta_max 0.989
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.650
_diffrn_reflns_Laue_measured_fraction_max 0.989
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_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_point_group_measured_fraction_full 0.650
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_diffrn_reflns_theta_max         21.752
_diffrn_reflns_theta_min         1.962
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1200
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_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.193
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7274
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_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0835
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1575P)^2^+5.7060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6261
_reflns_number_total             7274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00498f2.cif
_cod_data_source_block           DATA2a
_cod_original_cell_volume        3094.6(2)
_cod_database_code               4349868
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2013-4
_shelx_res_checksum              2607
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