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_7132131
_publ_section_title
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 Swift C--C Bond Insertion by a 12-Electron Palladium(0) Surrogate
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03964A
_journal_year                    2023
_chemical_formula_moiety         'C48 H62 N2 Pd, 2(C2.5 H2.5 N0.5)'
_chemical_formula_sum            'C53 H67 N3 Pd'
_chemical_formula_weight         852.49
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_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
_audit_creation_date             2018-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
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2023-08-11 deposited with the CCDC.	2023-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.994(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.1187(8)
_cell_length_b                   13.1872(6)
_cell_length_c                   32.3582(13)
_cell_measurement_reflns_used    9360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.38
_cell_volume                     8744.2(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX XT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            71739
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.094
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.464
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0428 before and 0.0393 after correction.
The Ratio of minimum to maximum transmission is 0.9512.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.824
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.474
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         9630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.474
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0660
_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^)+75.1704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9167
_reflns_number_total             9630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03964a2.cif
_cod_data_source_block           aag1807
_cod_database_code               7132131
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N100, C100}
{N200, C200}
3. Uiso/Uaniso restraints and constraints
Uanis(N100) = Uanis(C100)
Uanis(N200) = Uanis(C200)
4. Others
 Fixed Sof: N100(0.5) H100(0.5) C100(0.5) H10A(0.5) H101(0.5) H10B(0.5)
 H102(0.5) N200(0.5) C200(0.5) H200(0.5) H201(0.5) H20D(0.5) H202(0.5) H20E(0.5)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C31(H31), C34(H34)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C27(H27), C28(H28), C29(H29), C38(H38), C39(H39),
 C40(H40), C41(H41), C44(H44), C45(H45), C46(H46), C47(H47), N100(H100),
 C100(H10A), C101(H101), C101(H10B), C102(H102), C200(H200), C201(H201),
 C201(H20D), C202(H202), C202(H20E)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              20445
_shelx_hkl_checksum              89373
_olex2_submission_special_instructions 'No special instructions were received'