Polymerization of 1-chloro-2-phenylacetylene by cationic monoanionic tridentate (S,S)-bis(oxazolinylphenyl)amido-ligated palladium catalysts: is it a coordination‒insertion mechanism?
Wu, Xiaolu; Yang, Zhi; Yan, Xinwen; Zhang, Pengfei; Wang, Lin; Guo, Ge; Dong, Yuping; Li, Xiaofang; Polymer Chemistry 9 (2018) 4856–; doi:10.1039/C8PY00903A

data_1549868
_publ_section_title
;
 Polymerization of 1-chloro-2-phenylacetylene by cationic monoanionic
 tridentate (S,S)-bis(oxazolinylphenyl)amido-ligated palladium catalysts:
 is it a coordination--insertion mechanism?
;
_journal_issue                   39
_journal_name_full               'Polymer Chemistry'
_journal_page_first              4856
_journal_paper_doi               10.1039/C8PY00903A
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H20 Cl N3 O2 Pd'
_chemical_formula_sum            'C20 H20 Cl N3 O2 Pd'
_chemical_formula_weight         476.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-17 deposited with the CCDC.
2018-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.567(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7684(11)
_cell_length_b                   9.0383(9)
_cell_length_c                   10.8590(11)
_cell_measurement_reflns_used    5731
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      3.11
_cell_volume                     928.22(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8156
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         2.135
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.164
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.568
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 1372 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.032(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3250
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+3.7607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                3104
_reflns_number_total             3250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py00903a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1549868.cif.'
_cod_database_code               1549868
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.800
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.001 and
sigma for terminal atoms of 0.001
3.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C7(H7A,H7B)
3.c Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C)
3.d Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C12(H12), C18(H18), C11(H11), C20(H20), C13(H13), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'