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_4518627
_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
'C36 H37 N4 O3 P Pd, C H2 Cl2, C2.5 H7.5 O0.5'
_chemical_formula_sum            'C39.5 H46.5 Cl2 N4 O3.5 P Pd'
_chemical_formula_weight         841.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.686(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.848(2)
_cell_length_b                   18.223(3)
_cell_length_c                   16.659(3)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.010
_cell_measurement_theta_min      2.235
_cell_volume                     3844.8(11)
_computing_cell_refinement       'SAINT v8. 34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8. 34A (Bruker, 2013)'
_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      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35443
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.019
_diffrn_reflns_theta_min         1.669
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0596 before and 0.0409 after correction. The Ratio of minimum to maximum transmission is 0.9062. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1738
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9241
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0458P)^2^+7.6875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7499
_reflns_number_total             9241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00288_si_002.cif
_cod_data_source_block           12
_cod_original_cell_volume        3844.9(12)
_cod_original_formula_sum        'C39.50 H46.50 Cl2 N4 O3.50 P Pd'
_cod_database_code               4518627
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.901
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4S-C3S = C5S-C2S = C2S-C5T
 1.54 with sigma of 0.01
 O1S-C3S = O1S-C2S
 1.45 with sigma of 0.01
 C4S-O1S
 2.44 with sigma of 0.01
 O1S-C5S
 2.44 with sigma of 0.01
 O1S-C5T
 2.44 with sigma of 0.01
 C3S-C2S
 2.29 with sigma of 0.01
3. Rigid bond restraints
 C4S, C3S, O1S, C2S, C5S, C5T
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C4S \\sim C3S \\sim O1S \\sim C2S \\sim C5S \\sim C5T: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(H2SD)=Sof(H2SC)=Sof(C5T)=Sof(H5TA)=Sof(H5TB)=Sof(H5TC)=1-FVAR(1)
 Sof(H2SA)=Sof(H2SB)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=FVAR(1)
 Fixed Sof: C3S(0.5) H3SA(0.5) H3SB(0.5) O1S(0.5) C2S(0.5) C4S(0.5) H4SA(0.5)
 H4SC(0.5) H4SB(0.5)
6.a Ternary CH refined with riding coordinates:
 C34(H34), C33(H33)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C3S(H3SA,H3SB), C2S(H2SA,H2SB), C2S(H2SD,H2SC)
6.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C11(H11), C10(H10), C20(H20), C32(H32), C28(H28), C22(H22),
 C17(H17), C18(H18), C26(H26), C29(H29), C19(H19), C30(H30), C31(H31), C25(H25),
  C24(H24), C23(H23)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,
 H7B,H7C), C2(H2A,H2B,H2C), C4S(H4SA,H4SC,H4SB), C5S(H5SA,H5SB,H5SC), C5T(H5TA,
 H5TB,H5TC)
;
_shelx_res_checksum              86086
_shelx_hkl_checksum              51067
_olex2_submission_special_instructions 'No special instructions were received'