Air- and moisture-stable Xantphos-ligated palladium dialkyl complex as a precatalyst for cross-coupling reactions.
Takahashi, Rina; Kubota, Koji; Ito, Hajime; Chemical communications (Cambridge, England) 56 (2020) 407–410; doi:10.1039/c9cc06946a

data_7125642
_publ_section_title
;
 Air- and moisture-stable Xantphos-ligated palladium dialkyl complex as a
 precatalyst for cross-coupling reactions.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              407
_journal_page_last               410
_journal_paper_doi               10.1039/c9cc06946a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C47 H54 O P2 Pd Si2'
_chemical_formula_sum            'C47 H54 O P2 Pd Si2'
_chemical_formula_weight         859.42
_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     direct
_audit_creation_date             2019-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-18 deposited with the CCDC.	2019-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.720(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.6034(4)
_cell_length_b                   11.5855(2)
_cell_length_c                   35.7054(8)
_cell_measurement_reflns_used    39298
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.1650
_cell_measurement_theta_min      2.3390
_cell_volume                     8445.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -43.00   6.00   0.50   11.15    --    5.00  17.00-124.00   98
  2  \w     -8.00  17.00   0.50   11.15    --   -7.30  17.00-124.00   50
  3  \w     52.00  77.00   0.50   11.15    --    5.00  60.00  90.00   50
  4  \w    -23.00   3.00   0.50   11.15    --    5.00  60.00  90.00   52
  5  \w    -50.00 -24.00   0.50   11.15    --    5.00  60.00 150.00   52
  6  \w     11.00  37.00   0.50   11.15    --    5.00  60.00 150.00   52
  7  \w    -77.00 -51.00   0.50   11.15    --    5.00  60.00  90.00   52
  8  \w     14.00  64.00   0.50   11.15    --   -7.30  60.00-120.00  100
  9  \w    -97.00  -8.00   0.50   11.15    --   -7.30  60.00-120.00  178
 10  \w    -97.00  62.00   0.50   11.15    --   -7.30  43.00 150.00  318
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0107261000
_diffrn_orient_matrix_UB_12      -0.0145491000
_diffrn_orient_matrix_UB_13      -0.0174669000
_diffrn_orient_matrix_UB_21      0.0329161000
_diffrn_orient_matrix_UB_22      0.0098976000
_diffrn_orient_matrix_UB_23      0.0080405000
_diffrn_orient_matrix_UB_31      0.0029420000
_diffrn_orient_matrix_UB_32      -0.0586289000
_diffrn_orient_matrix_UB_33      0.0056729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            53737
_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         25.350
_diffrn_reflns_theta_min         2.138
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       plate
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         7717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0354P)^2^+19.6876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7014
_reflns_number_total             7717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06946a2.cif
_cod_data_source_block           tkh-1
_cod_depositor_comments          'Adding full bibliography for 7125642.cif.'
_cod_database_code               7125642
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C H O P Pd'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C42(H42A,H42B)
2.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C37(H37), C4(H4), C22(H22), C5(H5), C25(H25), C31(H31), C3(H3),
 C21(H21), C39(H39), C26(H26), C16(H16), C19(H19), C15(H15), C38(H38), C20(H20),
  C34(H34), C32(H32), C17(H17), C33(H33), C41(H41), C23(H23), C29(H29),
 C40(H40), C28(H28), C50(H50)
2.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C47(H47A,H47B,H47C), C45(H45A,H45B,
 H45C), C9(H9A,H9B,H9C), C43(H43A,H43B,H43C), C49(H49A,H49B,H49C), C10(H10A,
 H10B,H10C)
;
_shelx_res_checksum              2177
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.693
_oxdiff_exptl_absorpt_empirical_full_min 0.323