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_7705006
_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 H29 Cl2 F3 P2 Pd, 0.75(C4 H8 O)'
_chemical_formula_sum            'C43 H35 Cl2 F3 O0.75 P2 Pd'
_chemical_formula_weight         859.95
_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     dual
_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                 97.664(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.4249(10)
_cell_length_b                   9.8871(2)
_cell_length_c                   18.8438(5)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    210.1(3)
_cell_measurement_theta_max      27.9730
_cell_measurement_theta_min      3.3428
_cell_volume                     8018.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      210.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.829
_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     -9.00  87.00   0.75   48.14    --   12.36  19.00 -30.00  128
  2  \w    -12.00  55.50   0.75   48.14    --   12.36  19.00-120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0131143000
_diffrn_orient_matrix_UB_12      -0.0213866000
_diffrn_orient_matrix_UB_13      -0.0238617000
_diffrn_orient_matrix_UB_21      0.0085173000
_diffrn_orient_matrix_UB_22      -0.0565468000
_diffrn_orient_matrix_UB_23      -0.0099824000
_diffrn_orient_matrix_UB_31      -0.0052007000
_diffrn_orient_matrix_UB_32      -0.0386463000
_diffrn_orient_matrix_UB_33      0.0278052000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0817
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34635
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.600
_diffrn_reflns_theta_min         3.343
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         18695
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0754
_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^)+(0.0402P)^2^+22.2069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12003
_reflns_number_total             18695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02335c2.cif
_cod_data_source_block           11a
_cod_depositor_comments
'Adding full bibliography for 7705001--7705006.cif.'
_cod_database_code               7705006
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C63 H70 Cl2 F3 P2 Pd'
_chemical_oxdiff_usercomment     yellow
_reflns_odcompleteness_completeness 98.87
_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. Restrained distances
 C72-C75
 2.3 with sigma of 0.02
3. Others
 Fixed Sof: O71(0.5) C72(0.5) H72A(0.5) H72B(0.5) C73(0.5) H73A(0.5) H73B(0.5)
 C74(0.5) H74A(0.5) H74B(0.5) C75(0.5) H75A(0.5) H75B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C37A(H37A,H37B), C38A(H38A,H38B), C38B(H38C,H38D), C39B(H39A,H39B), C62(H62A,
 H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C72(H72A,H72B),
 C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B)
4.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C22A(H22A), C23A(H23A),
 C24A(H24A), C25A(H25A), C26A(H26A), C32A(H32A), C33A(H33A), C34A(H34A),
 C35A(H35A), C36A(H36A), C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A),
 C46A(H46A), C52A(H52A), C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A),
 C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C8B(H8B), C22B(H22B), C23B(H23B),
 C24B(H24B), C25B(H25B), C26B(H26B), C32B(H32B), C33B(H33B), C34B(H34B),
 C35B(H35B), C36B(H36B), C42B(H42B), C43B(H43B), C44B(H44B), C45B(H45B),
 C46B(H46B), C52B(H52B), C53B(H53B), C54B(H54B), C55B(H55B), C56B(H56B)
;
_shelx_res_checksum              60724
_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.901