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_7712477
_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         'C52 H70 As2 Cl2 O4 Pd, C H2 Cl2'
_chemical_formula_sum            'C53 H72 As2 Cl4 O4 Pd'
_chemical_formula_weight         1171.14
_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             2020-12-10
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-12-26 deposited with the CCDC.	2023-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                86.695(4)
_cell_angle_beta                 83.153(3)
_cell_angle_gamma                80.496(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8964(4)
_cell_length_b                   10.9483(5)
_cell_length_c                   23.1815(11)
_cell_measurement_reflns_used    7346
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      32.5780
_cell_measurement_theta_min      2.9250
_cell_volume                     2706.0(2)
_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 0.999
_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    -71.00 -44.00   0.30    2.50    --   30.00  54.00-120.00   90
  2  \w      7.00  32.80   0.30    2.50    --   30.00  54.00-120.00   86
  3  \w    -71.00  38.20   0.30    2.50    --   30.00  54.00 120.00  364
  4  \w    -73.00 108.80   0.30    2.50    --   30.00  54.00   0.00  606
;
_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      -0.0604632000
_diffrn_orient_matrix_UB_12      0.0219388000
_diffrn_orient_matrix_UB_13      0.0140230000
_diffrn_orient_matrix_UB_21      0.0201202000
_diffrn_orient_matrix_UB_22      -0.0224377000
_diffrn_orient_matrix_UB_23      0.0271934000
_diffrn_orient_matrix_UB_31      0.0187134000
_diffrn_orient_matrix_UB_32      0.0577634000
_diffrn_orient_matrix_UB_33      0.0038763000
_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  0.0226
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16790
_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         26.372
_diffrn_reflns_theta_min         2.638
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.521
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.622
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         11082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0246P)^2^+4.4326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9614
_reflns_number_total             11082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04139a2.cif
_cod_data_source_block           PdCl2(L6)2
_cod_database_code               7712477
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C106 H144 As4 Cl8 O8 Pd2 '
_shelx_estimated_absorpt_t_max   0.693
_shelx_estimated_absorpt_t_min   0.444
_diffrn_oxdiff_digest_frames
;
01876b9be41b3e852785dad73c8e4e15ec011465dad
;
_diffrn_oxdiff_digest_hkl
;
01ef15b569dc25178a73e3f595e08101f0e718
;
_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), C7(H7), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C15(H15A,H15B), C20(H20A,H20B), C16(H16A,H16B), C36(H36A,
 H36B), C37(H37A,H37B), C12(H12A,H12B), C32(H32A,H32B), C41(H41A,H41B),
 C17(H17A,H17B), C14(H14A,H14B), C13(H13A,H13B), C18(H18A,H18B), C19(H19A,H19B),
  C38(H38A,H38B), C39(H39A,H39B), C35(H35A,H35B), C33(H33A,H33B), C40(H40A,
 H40B), C53(H53A,H53B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C42(H42), C45(H45), C22(H22), C49(H49), C24(H24), C47(H47),
 C23(H23), C44(H44), C43(H43), C48(H48), C26(H26), C27(H27), C28(H28)
2.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56791
_shelx_hkl_checksum              59330
_shelx_fab_checksum              95946
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.890