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_7709287
_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            'C14 H32 Cl2 N2 O4 Pd'
_chemical_formula_weight         469.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 90.478(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0082(5)
_cell_length_b                   11.6508(8)
_cell_length_c                   18.8174(12)
_cell_measurement_reflns_used    9455
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.66
_cell_measurement_theta_min      4.15
_cell_volume                     1974.9(2)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37191
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         2.056
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.4674
_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    1.580
_exptl_crystal_description       lath
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.051
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+6.6809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3418
_reflns_number_total             4040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03778a2.cif
_cod_data_source_block           complex_1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7709287
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              64132
_shelx_hkl_checksum              93774