Homo- and copolymerization of norbornene using tridentate IzQO palladium catalysts with dimethylaminoethyl as a side arm
Dong, Jie; Wang, Baiquan; Polymer Chemistry 12 (2021) 4736–4747; doi:10.1039/D1PY00699A

data_1564312
_publ_section_title
;
 Homo- and copolymerization of norbornene using tridentate IzQO palladium
 catalysts with dimethylaminoethyl as a side arm
;
_journal_issue                   32
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4736
_journal_page_last               4747
_journal_paper_doi               10.1039/D1PY00699A
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C34 H38 Cl N3 O3 Pd, 0.13(C H2 Cl2)'
_chemical_formula_sum            'C34.12 H38.25 Cl1.25 N3 O3 Pd'
_chemical_formula_weight         689.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-05 deposited with the CCDC.	2021-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.780(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1028(7)
_cell_length_b                   14.4854(5)
_cell_length_c                   24.8028(9)
_cell_measurement_reflns_used    14409
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      32.1260
_cell_measurement_theta_min      1.7530
_cell_volume                     6367.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       CrystalClear(Rigaku,2008)
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -115.00  65.00   1.00    3.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00    3.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00    3.00    --  -25.00  45.00 180.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0030482000
_diffrn_orient_matrix_UB_12      -0.0431365000
_diffrn_orient_matrix_UB_13      -0.0128859000
_diffrn_orient_matrix_UB_21      -0.0238950000
_diffrn_orient_matrix_UB_22      -0.0203370000
_diffrn_orient_matrix_UB_23      0.0160599000
_diffrn_orient_matrix_UB_31      -0.0319687000
_diffrn_orient_matrix_UB_32      0.0111421000
_diffrn_orient_matrix_UB_33      -0.0207166000
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            33438
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         1.677
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             2842
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         6509
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0304P)^2^+13.3063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5311
_reflns_number_total             6509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py00699a2.cif
_cod_data_source_block           r20200914c
_cod_depositor_comments
'Adding full bibliography for 1564310--1564312.cif.'
_cod_database_code               1564312
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.874
_reflns_odcompleteness_completeness 99.91
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl3-C35 = Cl2-C35
 1.78 with sigma of 0.01
 Cl2-Cl3
 2.89 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Cl2(0.125) Cl3(0.125) C35(0.125) H35A(0.125) H35B(0.125)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C35(H35A,H35B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C30(H30),
 C32(H32), C33(H33)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C34(H34A,H34B,
 H34C)
;
_shelx_res_checksum              1962
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.327
_oxdiff_exptl_absorpt_empirical_full_min 0.793