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_7708917
_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(C24 H9 As Cl F18 Pd0.5), C H2 Cl2'
_chemical_formula_sum            'C49 H20 As2 Cl4 F36 Pd'
_chemical_formula_weight         1690.69
_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     iterative
_audit_creation_date             2021-03-30
_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                72.260(16)
_cell_angle_beta                 70.604(12)
_cell_angle_gamma                73.957(14)
_cell_formula_units_Z            2
_cell_length_a                   9.747(4)
_cell_length_b                   16.203(6)
_cell_length_c                   20.248(8)
_cell_measurement_reflns_used    8278
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.05
_cell_volume                     2817.7(19)
_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      93.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28964
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_min         3.047
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  0.603
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_description       block
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         12805
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0340P)^2^+3.8316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11754
_reflns_number_total             12805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02955j2.cif
_cod_data_source_block           1d-Pd
_cod_depositor_comments
'Adding full bibliography for 7708916--7708920.cif.'
_cod_original_cell_volume        2817.8(19)
_cod_database_code               7708917
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.460
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F32A-C47 \\sim F32B-C47
 with sigma of 0.02
 F4A-C10 \\sim F4B-C10
 with sigma of 0.02
 F6A-C10 \\sim F6B-C10
 with sigma of 0.02
 C10-F5A \\sim C10-F5B
 with sigma of 0.02
 F31A-C47 \\sim F31B-C47
 with sigma of 0.02
 C47-F33A \\sim C47-F33B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F5A \\sim F4B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.08
F4B \\sim F4A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) = Uanis(F4B)
4. Rigid body (RIGU) restrains
 F4B, F5B, F6B, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F33B, C47, F31B, F32B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F6A, F4A, F5A, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F32A, F31A, C47, F33A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(F31B)=Sof(F33B)=Sof(F32B)=1-FVAR(1)
 Sof(F32A)=Sof(F31A)=Sof(F33A)=FVAR(1)
 Sof(F5B)=Sof(F4B)=Sof(F6B)=1-FVAR(2)
 Sof(F6A)=Sof(F4A)=Sof(F5A)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C28(H28), C15(H15), C46(H46), C37(H37), C30(H30), C22(H22),
 C35(H35), C8(H8), C39(H39), C4(H4), C42(H42), C13(H13), C18(H18), C32(H32),
 C44(H44), C6(H6), C20(H20)
;
_shelx_res_checksum              51001
_shelx_hkl_checksum              17202
_olex2_submission_special_instructions 'No special instructions were received'