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_1559570
_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 Br2 Cl N2 Pd'
_chemical_formula_sum            'C41 H45 Br2 Cl N2 Pd'
_chemical_formula_weight         867.46
_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     direct
_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                 96.9770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8172(2)
_cell_length_b                   18.0795(3)
_cell_length_c                   16.7528(3)
_cell_measurement_reflns_used    6237
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.7900
_cell_measurement_theta_min      4.0870
_cell_volume                     3853.36(11)
_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    'SIR2004 (Burla et al., 2007)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.954
_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   -113.00 -20.00   1.00    2.19    --  -41.14 -38.00 120.00   93
  2  \w    -78.00  -2.00   1.00    2.19    --  -41.14 125.00 -60.00   76
  3  \w      2.00  66.00   1.00    2.19    --   41.14 -99.00 -60.00   64
  4  \w     81.00 170.00   1.00    8.78    --  110.65  77.00-150.00   89
  5  \w     99.00 178.00   1.00    8.78    --  110.65  30.00-180.00   79
  6  \w     82.00 173.00   1.00    8.78    --  110.65  61.00 -90.00   91
  7  \w     39.00 135.00   1.00    8.78    --  110.65 -61.00 120.00   96
;
_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      0.0556378000
_diffrn_orient_matrix_UB_12      0.0705185000
_diffrn_orient_matrix_UB_13      -0.0245836000
_diffrn_orient_matrix_UB_21      -0.1072849000
_diffrn_orient_matrix_UB_22      0.0340056000
_diffrn_orient_matrix_UB_23      -0.0317527000
_diffrn_orient_matrix_UB_31      -0.0080145000
_diffrn_orient_matrix_UB_32      0.0336350000
_diffrn_orient_matrix_UB_33      0.0834750000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13144
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.395
_diffrn_reflns_theta_min         3.611
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.173
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58714
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.594
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7604
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0953P)^2^+2.6026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6698
_reflns_number_total             7604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy01617a2.cif
_cod_data_source_block           18122603
_cod_depositor_comments
'Adding full bibliography for 1559569--1559575.cif.'
_cod_database_code               1559570
_chemical_oxdiff_formula         'C H N Br Pd Cl'
_chemical_oxdiff_usercomment     c4a
_reflns_odcompleteness_completeness 98.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.46
_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. Rigid bond restraints
 Cl1A, C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim C0AA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C1) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl1A) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C1(0.45) H1A(0.45) H1B(0.45) H1C(0.45) C0AA(0.55) H0AA(0.55)
 H0AB(0.55) H0AC(0.55) Cl1(0.55) Cl1A(0.45)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C11(H11), C13(H13), C17(H17), C20(H20), C30(H30)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C32(H32), C33(H33), C34(H34), C35(H35)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C0AA(H0AA,H0AB,H0AC), C31(H31A,H31B,H31C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C2(H2A,H2B,H2C)
;
_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 1.925
_oxdiff_exptl_absorpt_empirical_full_min 0.667