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_4132540
_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         'C33 H49 Cl N2 O3 P2 Pd'
_chemical_formula_sum            'C33 H49 Cl N2 O3 P2 Pd'
_chemical_formula_weight         725.58
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.858(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6631(6)
_cell_length_b                   21.6925(14)
_cell_length_c                   17.1226(10)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.8
_cell_volume                     3452.6(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.9975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31259
_diffrn_reflns_theta_full        27.5150
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0364 before and 0.0277 after correction.
The Ratio of minimum to maximum transmission is 0.9152.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.3958
_exptl_crystal_description       Block
_exptl_crystal_F_000             1509.9699
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5669
_refine_diff_density_min         -0.3886
_refine_diff_density_rms         0.0755
_refine_ls_d_res_high            0.7692
_refine_ls_d_res_low             13.1180
_refine_ls_goodness_of_fit_ref   1.0330
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    76
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0330
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.0013
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+3.9016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -12
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              -8
_reflns_number_gt                7537
_reflns_number_total             7933
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja8b04712_si_002.cif
_cod_data_source_block           mo_wz2_0m
_cod_database_code               4132540
_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 Ternary CH refined with riding coordinates and stretchable bonds:
 C32(H32), C29(H29), C26(H26), C23(H23)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C4(H4), C9(H9), C19(H19), C11(H11), C6(H6), C17(H17),
 C12(H12), C16(H16), C18(H18), C10(H10)
2.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C25(H25a,H25b,H25c), C31(H31a,H31b,H31c), C27(H27a,H27b,
 H27c), C28(H28a,H28b,H28c), C30(H30a,H30b,H30c), C24(H24a,H24b,H24c), C33(H33a,
 H33b,H33c), C14(H14a,H14b,H14c), C21(H21a,H21b,H21c), C1(H1a,H1b,H1c)
;