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_4132541
_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         'C22 H21 Cl O4 P Pd, C6 H16 N'
_chemical_formula_sum            'C28 H37 Cl N O4 P Pd'
_chemical_formula_weight         624.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_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                90
_cell_angle_beta                 98.316(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7229(4)
_cell_length_b                   15.9380(8)
_cell_length_c                   20.9835(11)
_cell_measurement_reflns_used    9254
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.73
_cell_measurement_theta_min      2.68
_cell_volume                     2886.6(2)
_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 0.9971
_diffrn_measured_fraction_theta_max 0.9967
_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  0.0220
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            61369
_diffrn_reflns_theta_full        30.7262
_diffrn_reflns_theta_max         30.73
_diffrn_reflns_theta_min         1.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0409 before and 0.0342 after correction.
The Ratio of minimum to maximum transmission is 0.9326.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4368
_exptl_crystal_description       block
_exptl_crystal_F_000             1285.5438
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.5543
_refine_diff_density_min         -0.3076
_refine_diff_density_rms         0.0782
_refine_ls_d_res_high            0.6955
_refine_ls_d_res_low             12.6427
_refine_ls_goodness_of_fit_ref   1.1425
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    59
_refine_ls_number_parameters     330
_refine_ls_number_reflns         8950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1425
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.0112
_refine_ls_shift/su_mean         0.0011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+1.9355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                8293
_reflns_number_total             8950
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja8b04712_si_002.cif
_cod_data_source_block           mo_CEP9_0m
_cod_original_cell_volume        2886.6(3)
_cod_database_code               4132541
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23a,H23b), C27(H27a,H27b), C25(H25a,H25b)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19), C20(H20),
 C13(H13), C12(H12), C11(H11), C10(H10)
2.d Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C28(H28a,H28b,H28c), C26(H26a,H26b,H26c), C22(H22a,H22b,
 H22c), C15(H15a,H15b,H15c), C1(H1a,H1b,H1c)
;