Structure and Gas-Phase Thermochemistry of a Pd/Cu Complex: Studies on a Model for Transmetalation Transition States.
Oeschger, Raphael J.; Chen, Peter; Journal of the American Chemical Society 139 (2017) 1069–1072; doi:10.1021/jacs.6b12152

data_4125503
_publ_section_title
;
 Structure and Gas-Phase Thermochemistry of a Pd/Cu Complex: Studies on a
 Model for Transmetalation Transition States.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1069
_journal_page_last               1072
_journal_paper_doi               10.1021/jacs.6b12152
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C26 H16 N2 Pd'
_chemical_formula_sum            'C26 H16 N2 Pd'
_chemical_formula_weight         462.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-29
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;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.921(10)
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_cell_length_a                   20.179(5)
_cell_length_b                   7.3128(18)
_cell_length_c                   24.983(6)
_cell_measurement_reflns_used    3868
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.29
_cell_volume                     3527.0(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'XS (Sheldrick, 2008)'
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_diffrn_detector                 'Bruker APEX2 area detector'
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_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Bruker/Nonius Kappa Apex2'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'double mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_av_unetI/netI     0.0989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31016
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         1.055
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms high brilliance'
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_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0989 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.9028.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       needle
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         8115
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0283P)^2^+0.2321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5627
_reflns_number_total             8115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b12152_si_004.cif
_cod_data_source_block           c260716_1_1_0m
_cod_depositor_comments          'Adding full bibliography for 4125503.cif.'
_cod_original_cell_volume        3527.1(15)
_cod_database_code               4125503
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 C19, C14, C18, C23, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C49(H49), C50(H50),
  C51(H51)
;
_shelx_res_checksum              81180
_shelx_hkl_checksum              80777
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-28
_olex2_date_sample_submission    2016-07-26
_olex2_submission_original_sample_id c260716_1_1
_olex2_submission_special_instructions 'No special instructions were received'