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_7708916
_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         'C36 H66 As2 Cl2 Pd'
_chemical_formula_sum            'C36 H66 As2 Cl2 Pd'
_chemical_formula_weight         826.02
_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             2021-03-04
_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                112.662(7)
_cell_angle_beta                 107.773(6)
_cell_angle_gamma                91.967(5)
_cell_formula_units_Z            1
_cell_length_a                   9.8187(6)
_cell_length_b                   10.2351(7)
_cell_length_c                   10.7679(10)
_cell_measurement_reflns_used    3741
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      32.3680
_cell_measurement_theta_min      3.3530
_cell_volume                     936.60(14)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'CCD area detector'
_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 0.998
_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     87.00 114.00   1.00    1.00    --   30.00  54.00 -60.00   27
  2  \w    -73.00  32.00   1.00    1.00    --   30.00  54.00-180.00  105
  3  \w    -73.00  33.00   1.00    1.00    --   30.00  54.00  60.00  106
  4  \w    -69.00  31.00   1.00    1.00    --   30.00  54.00 -60.00  100
;
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0235635000
_diffrn_orient_matrix_UB_12      -0.0345001000
_diffrn_orient_matrix_UB_13      0.0467500000
_diffrn_orient_matrix_UB_21      0.0099208000
_diffrn_orient_matrix_UB_22      -0.0593042000
_diffrn_orient_matrix_UB_23      -0.0564284000
_diffrn_orient_matrix_UB_31      0.0726525000
_diffrn_orient_matrix_UB_32      0.0332619000
_diffrn_orient_matrix_UB_33      0.0203868000
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5696
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.831
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.414
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
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    1.464
_exptl_crystal_description       prism
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0164P)^2^+0.5191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3415
_reflns_number_total             3830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02955j2.cif
_cod_data_source_block           1m-Pd
_cod_depositor_comments
'Adding full bibliography for 7708916--7708920.cif.'
_cod_original_cell_volume        936.60(13)
_cod_database_code               7708916
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Pd1Cl2As2C36H66
_shelx_estimated_absorpt_t_max   0.595
_shelx_estimated_absorpt_t_min   0.350
_diffrn_oxdiff_digest_frames
;
01c1a3dd57f70dcd9eb1b8e742a4ffdb860033846a6
;
_diffrn_oxdiff_digest_hkl
;
01b09f27be283d5dea91e4f6eb5cbdf219d450
;
_reflns_odcompleteness_completeness 99.84
_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
2.a Ternary CH refined with riding coordinates:
 C13(H13), C1(H1), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C12(H12A,H12B), C14(H14A,H14B), C8(H8A,H8B), C11(H11A,H11B),
 C10(H10A,H10B), C6(H6A,H6B), C15(H15A,H15B), C2(H2A,H2B), C5(H5A,H5B), C9(H9A,
 H9B), C3(H3A,H3B), C17(H17A,H17B), C4(H4A,H4B), C16(H16A,H16B)
;
_shelx_res_checksum              71007
_shelx_hkl_checksum              10698
_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 1.108
_oxdiff_exptl_absorpt_empirical_full_min 0.933