Electron-Rich Metal Cations Enable Synthesis of High Molecular Weight, Linear Functional Polyethylenes.
Zhang, Wei; Waddell, Peter M.; Tiedemann, Margaret A.; Padilla, Christian E.; Mei, Jiajun; Chen, Liye; Carrow, Brad P.; Journal of the American Chemical Society 140 (2018) 8841–8850; doi:10.1021/jacs.8b04712

data_4132537
_publ_section_title
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 Electron-Rich Metal Cations Enable Synthesis of High Molecular Weight,
 Linear Functional Polyethylenes.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8841
_journal_page_last               8850
_journal_paper_doi               10.1021/jacs.8b04712
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C23 H24 Cl O4 P Pd'
_chemical_formula_sum            'C23 H24 Cl O4 P Pd'
_chemical_formula_weight         537.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                104.785(1)
_cell_angle_beta                 100.092(1)
_cell_angle_gamma                106.757(1)
_cell_formula_units_Z            2
_cell_length_a                   8.9395(3)
_cell_length_b                   9.5963(4)
_cell_length_c                   14.4751(6)
_cell_measurement_reflns_used    9714
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.340
_cell_volume                     1107.37(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9988
_diffrn_measured_fraction_theta_max 0.9988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33201
_diffrn_reflns_theta_full        27.1674
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         2.34
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0484 before and 0.0335 after correction.
The Ratio of minimum to maximum transmission is 0.9522.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.6022
_exptl_crystal_description       columnar
_exptl_crystal_F_000             536.7455
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.8397
_refine_diff_density_min         -0.3645
_refine_diff_density_rms         0.0810
_refine_ls_d_res_high            0.7783
_refine_ls_d_res_low             8.7029
_refine_ls_goodness_of_fit_ref   1.0497
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4916
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0495
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+1.0919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -12
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4806
_reflns_number_total             4916
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja8b04712_si_002.cif
_cod_data_source_block           mo_CEP11_0m
_cod_database_code               4132537
_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.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C12(H12), C11(H11), C5(H5), C6(H6), C7(H7), C8(H8),
 C21(H21), C20(H20), C19(H19), C18(H18)
2.b Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C2(H2a,H2b,H2c), C23(H23a,H23b,H23c)
;