DMPDAB–Pd–MAH: A Versatile Pd(0) Source for Precatalyst Formation, Reaction Screening, and Preparative-Scale Synthesis
Huang, Jingjun; Isaac, Matthew; Watt, Ryan; Becica, Joseph; Dennis, Emma; Saidaminov, Makhsud I.; Sabbers, William A.; Leitch, David C.; ACS Catalysis  (2021) 5636–5646; doi:10.1021/acscatal.1c00288

data_4518623
_publ_section_title
;
 DMPDAB--Pd--MAH: A Versatile Pd(0) Source for Precatalyst Formation,
 Reaction Screening, and Preparative-Scale Synthesis
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              5636
_journal_page_last               5646
_journal_paper_doi               10.1021/acscatal.1c00288
_journal_year                    2021
_chemical_formula_moiety         'C40 H30 O4 P2 Pd, C4 H10 O'
_chemical_formula_sum            'C44 H40 O5 P2 Pd'
_chemical_formula_weight         817.10
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                99.623(2)
_cell_angle_beta                 106.450(2)
_cell_angle_gamma                105.981(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0488(7)
_cell_length_b                   12.4133(8)
_cell_length_c                   15.6581(10)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.868
_cell_measurement_theta_min      2.847
_cell_volume                     1908.8(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            75385
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.018
_diffrn_reflns_theta_min         2.537
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0852 before and 0.0663 after correction. The Ratio of minimum to maximum transmission is 0.8833. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         9217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0281P)^2^+4.2268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6594
_reflns_number_total             9217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00288_si_002.cif
_cod_data_source_block           3
_cod_database_code               4518623
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.913
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C42(H42A,H42B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C12(H12), C30(H30), C10(H10), C19(H19), C21(H21), C24(H24),
 C20(H20), C35(H35), C16(H16), C27(H27), C6(H6), C39(H39), C13(H13), C9(H9),
 C8(H8), C26(H26), C15(H15), C36(H36), C25(H25), C7(H7), C34(H34), C31(H31),
 C38(H38), C37(H37), C14(H14), C32(H32), C33(H33)
2.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              40888
_shelx_hkl_checksum              54760
_olex2_submission_special_instructions 'No special instructions were received'