Modulation of N^N'-bidentate chelating pyridyl-pyridylidene amide ligands offers mechanistic insights into Pd-catalysed ethylene/methyl acrylate copolymerisation.
Ó Máille, Gearóid M; Dall'Anese, Anna; Grossenbacher, Philipp; Montini, Tiziano; Milani, Barbara; Albrecht, Martin; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6133–6145; doi:10.1039/d1dt00389e

data_7707072
_publ_section_title
;
 Modulation of N^N'-bidentate chelating pyridyl-pyridylidene amide ligands
 offers mechanistic insights into Pd-catalysed ethylene/methyl acrylate
 copolymerisation.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6133
_journal_page_last               6145
_journal_paper_doi               10.1039/d1dt00389e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C20 H17 N4 O Pd, F6 P'
_chemical_formula_sum            'C20 H17 F6 N4 O P Pd'
_chemical_formula_weight         580.74
_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             2019-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-12 deposited with the CCDC.	2021-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                83.0730(10)
_cell_angle_beta                 81.0700(10)
_cell_angle_gamma                85.1350(10)
_cell_formula_units_Z            2
_cell_length_a                   7.76590(10)
_cell_length_b                   11.65990(10)
_cell_length_c                   11.85750(10)
_cell_measurement_reflns_used    17409
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      76.3710
_cell_measurement_theta_min      3.7890
_cell_volume                     1050.542(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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      173.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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     32.00 120.00   0.50    0.10    --   47.95  60.00  13.00  176
  2  \w    -23.00  64.00   0.50    0.10    --   47.95 -60.00-125.00  174
  3  \w     92.00 174.00   0.50    0.39    --  107.11  60.00  13.00  164
  4  \w     36.00  67.00   0.50    0.39    --  107.11 -60.00-125.00   62
  5  \w    -34.00  54.00   0.50    0.10    --  -18.75  60.00  13.00  176
  6  \w    -90.00  -2.00   0.50    0.10    --  -18.75 -60.00-125.00  176
  7  \w    -66.00  -9.00   0.50    0.10    --  -18.75 125.00  60.00  114
  8  \w    -66.00  -9.00   0.50    0.10    --  -18.75 125.00  30.00  114
  9  \w    -26.00  23.00   0.50    0.10    --   47.95 -19.00 120.00   98
 10  \w    -26.00  23.00   0.50    0.10    --   47.95 -19.00  90.00   98
 11  \w     32.00  96.00   0.50    0.10    --   47.95-125.00  90.00  128
 12  \w     95.00 174.00   0.50    0.39    --  107.11  45.00  60.00  158
 13  \w     35.00 102.00   0.50    0.39    --  107.11 -77.00 -30.00  134
 14  \w     35.00 102.00   0.50    0.39    --  107.11 -77.00  60.00  134
 15  \w     35.00  68.00   0.50    0.39    --  107.11 -61.00  60.00   66
 16  \w     35.00 109.00   0.50    0.39    --  107.11 -94.00-180.00  148
 17  \w     35.00  68.00   0.50    0.39    --  107.11 -61.00 -30.00   66
 18  \w     35.00 117.00   0.50    0.39    --  107.11-125.00 -60.00  164
 19  \w     94.00 174.00   0.50    0.39    --  107.11  15.00 -90.00  160
 20  \w     35.00  68.00   0.50    0.39    --  107.11 -61.00  90.00   66
 21  \w     35.00 117.00   0.50    0.39    --  107.11-125.00-180.00  164
 22  \w     91.00 174.00   0.50    0.39    --  107.11  61.00  30.00  166
 23  \w     95.00 174.00   0.50    0.39    --  107.11  45.00 -30.00  158
 24  \w     35.00 109.00   0.50    0.39    --  107.11 -94.00 -30.00  148
 25  \w     35.00 109.00   0.50    0.39    --  107.11 -94.00  60.00  148
 26  \w     95.00 174.00   0.50    0.39    --  107.11  30.00-180.00  158
 27  \w     35.00 117.00   0.50    0.39    --  107.11-125.00-120.00  164
 28  \w     35.00 109.00   0.50    0.39    --  107.11 -94.00 -60.00  148
 29  \w     35.00 109.00   0.50    0.39    --  107.11 -94.00-120.00  148
 30  \w     95.00 174.00   0.50    0.39    --  107.11  45.00 -60.00  158
 31  \w    -66.00  -9.00   0.50    0.10    --  -18.75 125.00-120.00  114
 32  \w     26.00 120.00   0.50    0.10    --   47.95  77.00  60.00  188
 33  \w     26.00 120.00   0.50    0.10    --   47.95  77.00  30.00  188
 34  \w     26.00 120.00   0.50    0.10    --   47.95  77.00-150.00  188
 35  \w    -26.00  23.00   0.50    0.10    --   47.95 -19.00 -60.00   98
 36  \w     26.00 120.00   0.50    0.10    --   47.95  77.00 -60.00  188
 37  \w     26.00 120.00   0.50    0.10    --   47.95  77.00-180.00  188
 38  \w     26.00 120.00   0.50    0.10    --   47.95  77.00 -90.00  188
 39  \w     26.00 101.00   0.50    0.10    --   47.95  77.00 150.00  150
 40  \w     26.00 120.00   0.50    0.10    --   47.95  77.00 120.00  188
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1712876000
_diffrn_orient_matrix_UB_12      -0.0194781000
_diffrn_orient_matrix_UB_13      0.0521320000
_diffrn_orient_matrix_UB_21      0.0633398000
_diffrn_orient_matrix_UB_22      -0.0963453000
_diffrn_orient_matrix_UB_23      -0.0779296000
_diffrn_orient_matrix_UB_31      0.0845975000
_diffrn_orient_matrix_UB_32      0.0901868000
_diffrn_orient_matrix_UB_33      -0.0933525000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20226
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.165
_diffrn_reflns_theta_min         3.796
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.543
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.305
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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    1.836
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0386P)^2^+2.2112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4260
_reflns_number_total             4327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00389e2.cif
_cod_data_source_block           19ma080_pg010
_cod_depositor_comments          'Adding full bibliography for 7707072.cif.'
_cod_database_code               7707072
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C20 H17 F6 N4 O P Pd '
_chemical_oxdiff_usercomment     PG010
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.267
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C17(H17)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              9087
_shelx_hkl_checksum              35821
_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 1.505
_oxdiff_exptl_absorpt_empirical_full_min 0.732