Steric and electronic effects of arsa-Buchwald ligands on Suzuki-Miyaura coupling reaction.
Sumida, Akifumi; Ogawa, Kenta; Imoto, Hiroaki; Naka, Kensuke; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2838–2844; doi:10.1039/d2dt04139a

data_7712478
_publ_section_title
;
 Steric and electronic effects of arsa-Buchwald ligands on Suzuki-Miyaura
 coupling reaction.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2838
_journal_page_last               2844
_journal_paper_doi               10.1039/d2dt04139a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C48 H62 As2 Cl2 O4 Pd, 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H66 As2 Cl6 O4 Pd'
_chemical_formula_weight         1199.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-04
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2022-12-26 deposited with the CCDC.	2023-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                83.456(4)
_cell_angle_beta                 63.747(6)
_cell_angle_gamma                80.103(5)
_cell_formula_units_Z            1
_cell_length_a                   11.4318(8)
_cell_length_b                   11.5359(5)
_cell_length_c                   11.5689(6)
_cell_measurement_reflns_used    2919
_cell_measurement_temperature    77
_cell_measurement_theta_max      31.0570
_cell_measurement_theta_min      2.9610
_cell_volume                     1346.68(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      77
_diffrn_detector                 'CCD plate'
_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     90.00 116.00   0.40    2.50    --   30.00  54.00 -60.00   65
  2  \w    -73.00  33.00   0.40    2.50    --   30.00  54.00-180.00  265
  3  \w    -71.00  33.00   0.40    2.50    --   30.00  54.00  60.00  260
  4  \w    -67.00  34.20   0.40    2.50    --   30.00  54.00 -60.00  253
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0324015000
_diffrn_orient_matrix_UB_12      -0.0062065000
_diffrn_orient_matrix_UB_13      0.0682399000
_diffrn_orient_matrix_UB_21      0.0604468000
_diffrn_orient_matrix_UB_22      -0.0255089000
_diffrn_orient_matrix_UB_23      0.0013752000
_diffrn_orient_matrix_UB_31      0.0131613000
_diffrn_orient_matrix_UB_32      0.0566887000
_diffrn_orient_matrix_UB_33      0.0048515000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8205
_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         26.371
_diffrn_reflns_theta_min         2.532
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.902
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.480
_exptl_crystal_description       plate
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.549
_exptl_crystal_size_mid          0.327
_exptl_crystal_size_min          0.252
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0268P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4320
_reflns_number_total             5513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04139a2.cif
_cod_data_source_block           PdCl2(L11)2
_cod_database_code               7712478
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOAsPdCl
_shelx_estimated_absorpt_t_max   0.646
_shelx_estimated_absorpt_t_min   0.422
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C8(H8A,H8B), C4(H4A,H4B), C9(H9A,H9B), C10(H10A,
 H10B), C6(H6A,H6B), C5(H5A,H5B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C19(H19), C14(H14), C20(H20), C21(H21)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.816