Swift C–C Bond Insertion by a 12-Electron Palladium(0) Surrogate
Breitwieser, Kevin; Dankert, Fabian; Gruenwald, Annette; Mayer, Paula R.; Heinemann, Frank; Munz, Dominik; Chemical Communications  (2023) –; doi:10.1039/D3CC03964A

data_7132127
_publ_section_title
;
 Swift C--C Bond Insertion by a 12-Electron Palladium(0) Surrogate
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03964A
_journal_year                    2023
_chemical_formula_moiety         'C47 H62 N2 Pd, 2(C6 H6)'
_chemical_formula_sum            'C59 H74 N2 Pd'
_chemical_formula_weight         917.60
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-08-11 deposited with the CCDC.	2023-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2411(12)
_cell_length_b                   18.2386(11)
_cell_length_c                   32.1839(18)
_cell_measurement_reflns_used    2397
_cell_measurement_temperature    152.65
_cell_measurement_theta_max      18.721
_cell_measurement_theta_min      2.321
_cell_volume                     10120.3(11)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      152.65
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.2177
_diffrn_reflns_av_unetI/netI     0.2252
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37672
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         24.500
_diffrn_reflns_theta_min         1.265
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0792 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.7962.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       needle
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.880
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.2131
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0485P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3517
_reflns_number_total             8384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03964a2.cif
_cod_data_source_block           stru4963_0m
_cod_database_code               7132127
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.888
_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:
 C22(H22), C19(H19), C34(H34), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C29(H29), C28(H28), C27(H27), C40(H40),
 C44(H44), C45(H45), C46(H46), C47(H47), C43(H43), C55(H55), C54(H54), C59(H59),
  C58(H58), C57(H57), C56(H56), C50(H50), C49(H49), C48(H48), C53(H53),
 C52(H52), C51(H51)
2.d Fitted hexagon refined as free rotating group:
 C55(C54,C59,C58,C57,C56), C50(C49,C48,C53,C52,C51)
2.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C20(H20A,H20B,
 H20C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              48668
_shelx_hkl_checksum              27036
_olex2_submission_special_instructions 'No special instructions were received'