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_4518624
_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         'C43 H34 O4 P2 Pd, C0.5 H Cl'
_chemical_formula_sum            'C43.5 H35 Cl O4 P2 Pd'
_chemical_formula_weight         825.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.779(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7326(18)
_cell_length_b                   13.2010(8)
_cell_length_c                   23.4604(17)
_cell_measurement_reflns_used    5213
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.819
_cell_measurement_theta_min      2.33
_cell_volume                     7113.0(9)
_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      99.99
_diffrn_measured_fraction_theta_full 0.999
_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  0.0645
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.973
_diffrn_reflns_theta_min         1.773
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7068
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0589 before and 0.0516 after correction. The Ratio of minimum to maximum transmission is 0.9480. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       needle
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         8524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0288P)^2^+15.3152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6402
_reflns_number_total             8524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00288_si_002.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C43.50 H35 Cl O4 P2 Pd'
_cod_database_code               4518624
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.898
_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. Others
 Fixed Sof: H44A(0.5) H44B(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B)
3.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C12(H12), C16(H16), C22(H22), C6(H6), C37(H37), C10(H10), C31(H31),
 C39(H39), C24(H24), C19(H19), C32(H32), C27(H27), C8(H8), C28(H28), C9(H9),
 C26(H26), C15(H15), C13(H13), C38(H38), C18(H18), C14(H14), C25(H25), C20(H20),
  C7(H7), C21(H21)
3.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              93585
_shelx_hkl_checksum              32394
_olex2_submission_special_instructions 'No special instructions were received'