Experimental study of speciation and mechanistic implications when using chelating ligands in aryl-alkynyl Stille coupling.
Gallego, Ana M.; Peñas-Defrutos, Marconi N; Marcos-Ayuso, Guillermo; Martin-Alvarez, Jose M; Martínez-Ilarduya, Jesús M; Espinet, Pablo; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11336–11345; doi:10.1039/d0dt02335c

data_7705002
_publ_section_title
;
 Experimental study of speciation and mechanistic implications when using
 chelating ligands in aryl-alkynyl Stille coupling.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11336
_journal_page_last               11345
_journal_paper_doi               10.1039/d0dt02335c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C40 H28 Cl3 F3 Fe P2 Pd'
_chemical_formula_sum            'C40 H28 Cl3 F3 Fe P2 Pd'
_chemical_formula_weight         896.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-28 deposited with the CCDC.	2020-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.932(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2042(4)
_cell_length_b                   19.5582(5)
_cell_length_c                   14.3252(4)
_cell_measurement_reflns_used    5730
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.3930
_cell_measurement_theta_min      3.7420
_cell_volume                     3605.66(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      296.15
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.854
_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    -31.00  58.00   1.00   45.42    --  -10.64  19.00 -60.00   89
  2  \w     16.00  43.00   1.00   45.42    --  -10.64  19.00  90.00   27
  3  \w    -46.00   8.00   1.00   45.42    --  -10.64  19.00  90.00   54
  4  \w     58.00  99.00   1.00   45.42    --   12.20-178.00 120.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0623
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19703
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.549
_diffrn_reflns_theta_min         3.333
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.651
_exptl_crystal_description       prism
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+1.6378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5929
_reflns_number_total             8618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02335c2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7705001--7705006.cif.'
_cod_database_code               7705002
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
  C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63),
 C64(H64), C65(H65), C67(H67), C68(H68), C69(H69), C70(H70)
;
_shelx_res_checksum              13657
_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
;