Combining hydrogen bonding interactions with steric and electronic modifications for thermally robust α-diimine palladium catalysts toward ethylene (co)polymerization
Zheng, Handou; Zhong, Liu; Du, Cheng; Du, Wenbo; Cheung, Chi Shing; Ruan, Jingjing; Gao, Haiyang; Catalysis Science & Technology 11 (2021) 124–135; doi:10.1039/D0CY01617A

data_1559575
_publ_section_title
;
 Combining hydrogen bonding interactions with steric and electronic
 modifications for thermally robust \a-diimine palladium catalysts toward
 ethylene (co)polymerization
;
_journal_issue                   1
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              124
_journal_page_last               135
_journal_paper_doi               10.1039/D0CY01617A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C41 H45 Cl I2 N2 Pd'
_chemical_formula_sum            'C41 H45 Cl I2 N2 Pd'
_chemical_formula_weight         961.44
_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     iterative
_audit_creation_date             2020-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2020-08-04 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.055(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0308(2)
_cell_length_b                   19.7307(4)
_cell_length_c                   20.2309(4)
_cell_measurement_reflns_used    22788
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.3240
_cell_measurement_theta_min      3.6940
_cell_volume                     3929.69(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.927
_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    -20.00  48.00   1.00   37.50    --    7.28 -99.00 -30.00   68
  2  \w    -25.00  83.00   1.00   37.50    --    7.28  77.00 120.00  108
  3  \w    -17.00  82.00   1.00   37.50    --    7.28  38.00  30.00   99
  4  \w    -31.00  68.00   1.00   37.50    --   -6.11  38.00  90.00   99
  5  \w    -20.00  35.00   1.00   37.50    --   -6.11 -99.00-180.00   55
  6  \w    -67.00  32.00   1.00   37.50    --    7.28 -38.00   0.00   99
  7  \w    -67.00  18.00   1.00   37.50    --    7.28 -38.00-150.00   85
  8  \w     11.00  72.00   1.00   37.50    --    7.28-140.00-128.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0041853000
_diffrn_orient_matrix_UB_12      -0.0354074000
_diffrn_orient_matrix_UB_13      -0.0053239000
_diffrn_orient_matrix_UB_21      -0.0121182000
_diffrn_orient_matrix_UB_22      0.0054475000
_diffrn_orient_matrix_UB_23      -0.0352970000
_diffrn_orient_matrix_UB_31      0.0709071000
_diffrn_orient_matrix_UB_32      0.0030061000
_diffrn_orient_matrix_UB_33      0.0012386000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68625
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.966
_diffrn_reflns_theta_min         3.181
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.625
_exptl_crystal_description       needle
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.030
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8763
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0370P)^2^+12.6467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7037
_reflns_number_total             8763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy01617a2.cif
_cod_data_source_block           19030706
_cod_depositor_comments
'Adding full bibliography for 1559569--1559575.cif.'
_cod_database_code               1559575
_chemical_oxdiff_formula         CHNPdClI
_chemical_oxdiff_usercomment     Pd-I
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(Cl1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1A) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) = Uanis(Cl1A)
Uanis(C1A) = Uanis(Cl1)
3. Others
 Fixed Sof: C1A(0.35) H1AA(0.35) H1AB(0.35) H1AC(0.35) Cl1A(0.35) C1(0.65)
 H1A(0.65) H1B(0.65) H1C(0.65) Cl1(0.65)
4.a Ternary CH refined with riding coordinates:
 C5(H5), C10(H10), C21(H21), C22(H22), C28(H28), C31(H31)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C17(H17), C19(H19), C20(H20), C24(H24), C26(H26),
 C27(H27), C29(H29), C30(H30), C32(H32), C33(H33)
4.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C1(H1A,H1B,H1C)
;
_shelx_shelxl_version_number     2014/7
_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 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.556