Tertiary arsine ligands for the Stille coupling reaction.
Chishiro, Akane; Konishi, Masafumi; Inaba, Ryoto; Yumura, Takashi; Imoto, Hiroaki; Naka, Kensuke; Dalton transactions (Cambridge, England : 2003) 51 (2021) 95–103; doi:10.1039/d1dt02955j

data_7708918
_publ_section_title
;
 Tertiary arsine ligands for the Stille coupling reaction.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              95
_journal_page_last               103
_journal_paper_doi               10.1039/d1dt02955j
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         '2(C18 H15 As Cl Pd0.5)'
_chemical_formula_sum            'C36 H30 As2 Cl2 Pd'
_chemical_formula_weight         789.74
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-03
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-06-01 deposited with the CCDC.	2021-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.131(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1460(14)
_cell_length_b                   20.0852(19)
_cell_length_c                   10.5283(10)
_cell_measurement_reflns_used    1450
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1090
_cell_measurement_theta_min      2.4370
_cell_volume                     3200.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.83
_diffrn_detector_type            'Rigaku Mercury area detector'
_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    -73.00 111.00   0.50   12.00    --   30.00  54.00-180.00  368
  2  \w    -24.00  21.00   0.50   12.00    --   30.00  54.00 -30.00   90
;
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.1511
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12849
_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         26.370
_diffrn_reflns_theta_min         2.434
_exptl_absorpt_coefficient_mu    2.823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       cube
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0290P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3609
_reflns_number_total             6539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02955j2.cif
_cod_data_source_block           AsPh3-Pd
_cod_depositor_comments
'Adding full bibliography for 7708916--7708920.cif.'
_cod_database_code               7708918
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C32(H32), C2(H2), C18(H18), C33(H33), C26(H26), C14(H14), C34(H34),
 C10(H10), C35(H35), C8(H8), C11(H11), C12(H12), C15(H15), C30(H30), C24(H24),
 C9(H9), C27(H27), C3(H3), C20(H20), C28(H28), C16(H16), C17(H17), C29(H29),
 C6(H6), C23(H23), C22(H22), C4(H4), C21(H21), C5(H5)
;
_shelx_res_checksum              30683
_shelx_hkl_checksum              30502
_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
;