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_1564310
_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         'C18 H26 Cl N3 O Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C18.5 H27 Cl2 N3 O Pd'
_chemical_formula_weight         484.73
_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             2020-07-20
_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                62.136(5)
_cell_angle_beta                 84.247(4)
_cell_angle_gamma                84.451(4)
_cell_formula_units_Z            4
_cell_length_a                   9.5481(5)
_cell_length_b                   15.1927(7)
_cell_length_c                   15.9838(8)
_cell_measurement_reflns_used    12069
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      32.8240
_cell_measurement_theta_min      2.4730
_cell_volume                     2036.2(2)
_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    2.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00    2.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00    2.00    --  -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      -0.0631837000
_diffrn_orient_matrix_UB_12      -0.0147436000
_diffrn_orient_matrix_UB_13      -0.0084491000
_diffrn_orient_matrix_UB_21      0.0013032000
_diffrn_orient_matrix_UB_22      0.0408201000
_diffrn_orient_matrix_UB_23      -0.0463022000
_diffrn_orient_matrix_UB_31      0.0399837000
_diffrn_orient_matrix_UB_32      -0.0302355000
_diffrn_orient_matrix_UB_33      -0.0177272000
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21597
_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         26.372
_diffrn_reflns_theta_min         2.494
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         8298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0299P)^2^+0.4776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6704
_reflns_number_total             8298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py00699a2.cif
_cod_data_source_block           r20200709d_sq
_cod_depositor_comments
;
Adding full bibliography for 1564310--1564312.cif.

2022-04-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C37 H54 Cl4 N6 O2 Pd2'
_cod_original_formula_weight         969.46
_cod_original_formula_moiety         '2(C18 H26 Cl N3 O Pd), C H2 Cl2'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2036.21(19)
_cod_database_code               1564310
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.797
_reflns_odcompleteness_completeness 99.89
_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.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C33(H33A,H33B), C34(H34A,H34B), C37(H37A,H37B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C13(H13), C14(H14), C21(H21), C25(H25), C31(H31), C32(H32)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_shelx_res_checksum              35227
_shelx_fab_checksum              70667
_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 2.274
_oxdiff_exptl_absorpt_empirical_full_min 0.511