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_4518625
_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         'C38 H30 Fe O3 P2 Pd'
_chemical_formula_sum            'C38 H30 Fe O3 P2 Pd'
_chemical_formula_weight         758.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 124.36(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.339(12)
_cell_length_b                   8.380(4)
_cell_length_c                   17.649(9)
_cell_measurement_reflns_used    9677
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.60
_cell_volume                     3216(3)
_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 0.993
_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  0.1286
_diffrn_reflns_av_unetI/netI     0.1243
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52738
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.109
_diffrn_reflns_theta_min         2.605
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0922 before and 0.0741 after correction. The Ratio of minimum to maximum transmission is 0.8718. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.556
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7730
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.1147
_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^)+(0.0368P)^2^+21.0261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.984
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                5689
_reflns_number_total             7730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00288_si_002.cif
_cod_data_source_block           5
_cod_database_code               4518625
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(6)
 0.06(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C28(H28), C23(H23), C25(H25), C34(H34), C32(H32), C38(H38),
 C26(H26), C12(H12), C37(H37), C8(H8), C7(H7), C21(H21), C24(H24), C29(H29),
 C31(H31), C6(H6), C9(H9), C18(H18), C15(H15), C19(H19), C14(H14), C35(H35),
 C30(H30), C36(H36), C20(H20), C16(H16), C13(H13)
;
_shelx_res_checksum              9743
_shelx_hkl_checksum              6718
_olex2_submission_special_instructions 'No special instructions were received'