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_4132538
_publ_section_title
;
 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         'C25 H31 Cl O5 P2 Pd'
_chemical_formula_sum            'C25 H31 Cl O5 P2 Pd'
_chemical_formula_weight         615.34
_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             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                 103.122(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8242(3)
_cell_length_b                   18.5471(6)
_cell_length_c                   16.3705(6)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.36
_cell_measurement_theta_min      3.66
_cell_volume                     2609.29(16)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9696
_diffrn_measured_fraction_theta_max 0.9696
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28020
_diffrn_reflns_theta_full        72.3607
_diffrn_reflns_theta_max         72.36
_diffrn_reflns_theta_min         3.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.123
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0664 before and 0.0404 after correction.
The Ratio of minimum to maximum transmission is 0.7866.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.5663
_exptl_crystal_description       columnar
_exptl_crystal_F_000             1263.6956
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.071
_refine_diff_density_max         2.2082
_refine_diff_density_min         -1.1535
_refine_diff_density_rms         0.1311
_refine_ls_d_res_high            0.8089
_refine_ls_d_res_low             12.0902
_refine_ls_goodness_of_fit_ref   1.0394
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5005
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0388
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+13.5857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -10
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              -7
_reflns_number_gt                4816
_reflns_number_total             5005
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja8b04712_si_002.cif
_cod_data_source_block           cu_cep12_0m
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4132538
_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:
 C4(H4a,H4b), C2(H2a,H2b)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C13(H13), C10(H10), C8(H8), C21(H21), C23(H23), C7(H7), C14(H14),
 C22(H22), C15(H15), C16(H16), C9(H9)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C25(H25a,H25b,H25c), C18(H18a,H18b,H18c), C5(H5a,H5b,H5c),
 C3(H3a,H3b,H3c)
;