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_4518622
_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         'C22 H22 N2 O3 Pd'
_chemical_formula_sum            'C22 H22 N2 O3 Pd'
_chemical_formula_weight         468.81
_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_date             2020-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                70.989(2)
_cell_angle_beta                 70.567(2)
_cell_angle_gamma                71.163(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1137(9)
_cell_length_b                   10.2220(10)
_cell_length_c                   12.2985(12)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.44
_cell_volume                     991.53(17)
_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)'
_diffrn_ambient_temperature      99.96
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.984
_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  0.0136
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16832
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.074
_diffrn_reflns_theta_min         1.811
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0483 before and 0.0227 after correction. The Ratio of minimum to maximum transmission is 0.9350. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0162
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+0.6548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4591
_reflns_number_total             4746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00288_si_002.cif
_cod_data_source_block           1
_cod_database_code               4518622
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.533
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20), C19(H19)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C5(H5), C6(H6), C15(H15), C7(H7), C17(H17), C16(H16)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              29631
_shelx_hkl_checksum              61359
_olex2_submission_special_instructions 'No special instructions were received'