Quadrol-Pd(II) complexes: phosphine-free precatalysts for the room-temperature Suzuki-Miyaura synthesis of nucleoside analogues in aqueous media
Serrano, Jose Luis; Gaware, Sujeet; Pérez de Haro, Jose Antonio; Pérez, Jose; Lozano, Pedro; Kori, Santosh; Dandela, Rambabu; Sanghvi, Yogesh S.; Kapdi, Anant R.; Dalton Transactions  (2022) –; doi:10.1039/D1DT03778A

data_7709286
_publ_section_title
;
 Quadrol-Pd(II) complexes: phosphine-free precatalysts for the
 room-temperature Suzuki-Miyaura synthesis of nucleoside analogues in
 aqueous media
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03778A
_journal_year                    2022
_chemical_formula_sum            'C31 H48 N4 O12 Pd S2'
_chemical_formula_weight         839.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2bc 2ac'
_space_group_name_H-M_alt        'P c a b'
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-01-06 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.7548(7)
_cell_length_b                   14.9919(8)
_cell_length_c                   33.9400(17)
_cell_measurement_reflns_used    9478
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.28
_cell_volume                     7507.6(7)
_computing_data_collection       'APEX3 2019.1_0 (Bruker AXS Inc.)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            158800
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_min         2.027
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.989
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         11463
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0420P)^2^+28.0205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9683
_reflns_number_total             11463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03778a2.cif
_cod_data_source_block           complex_3
_cod_database_code               7709286
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              90121
_shelx_hkl_checksum              52570