Ultra-high molecular weight elastomeric polyethylene using an electronically and sterically enhanced nickel catalyst
Mahmood, Qaiser; Zemg, Yanning; Yue, Erlin; Solan, Gregory; Liang, Tongling; Sun, Wen Hua; Polym. Chem.  (2017) –; doi:10.1039/C7PY01606A

data_1547496
_publ_section_title
;
 Ultra-high molecular weight elastomeric polyethylene using an
 electronically and sterically enhanced nickel catalyst
;
_journal_name_full               'Polym. Chem.'
_journal_paper_doi               10.1039/C7PY01606A
_journal_year                    2017
_chemical_formula_moiety         'C58 H52 Br2 N2 Ni'
_chemical_formula_sum            'C58 H52 Br2 N2 Ni'
_chemical_formula_weight         995.54
_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             2017-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-06-01 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.09(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.452(2)
_cell_length_b                   19.191(4)
_cell_length_c                   12.944(3)
_cell_measurement_reflns_used    8121
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4839
_cell_measurement_theta_min      1.5731
_cell_volume                     2595.9(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.1053
              2theta: -19.8610
scan:
    Number of images: 342
               Slice: -110.0000 - 61.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.1053
              2theta: -19.8610
scan:
    Number of images: 280
               Slice: -79.0000 - 61.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.1053
              2theta: -19.8610
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27884
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.528
_exptl_absorpt_coefficient_mu    1.950
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8162
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.435
_exptl_crystal_size_min          0.211
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 4374 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         11768
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.5730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                10956
_reflns_number_total             11768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7py01606a2.cif
_cod_data_source_block           Ni2
_cod_original_cell_volume        2595.8(9)
_cod_database_code               1547496
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29I-C27I = C27-C29 = C27-C30 = C28-C27 = C28I-C27I = C27I-C30I
 1.54 with sigma of 0.01
 C29I-C30I
 2.5 with sigma of 0.02
 C28I-C29I
 2.5 with sigma of 0.02
 C28I-C30I
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C30 \\sim C29 \\sim C27I \\sim C28I \\sim C29I \\sim C30I:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C58I \\sim C58: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C27I) \\sim Ueq, Uanis(C28I) \\sim Ueq, Uanis(C29I) \\sim Ueq,
Uanis(C30I) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C58I) \\sim Ueq, Uanis(C58) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C27I)=Sof(C28I)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29I)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=Sof(C30I)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
 Sof(H19C)=Sof(H19D)=Sof(C58I)=Sof(H58D)=Sof(H58E)=Sof(H58F)=1-FVAR(2)
 Sof(H19A)=Sof(H19B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C31(H31), C44(H44)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C19(H19A,H19B), C19(H19C,H19D)
5.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C4(H4), C25(H25), C33(H33), C39(H39), C23(H23), C3(H3), C10(H10),
 C43(H43), C50(H50), C37(H37), C8(H8), C40(H40), C53(H53), C17(H17), C5(H5),
 C56(H56), C49(H49), C35(H35), C55(H55), C54(H54), C47(H47), C42(H42), C16(H16),
  C15(H15), C9(H9), C46(H46), C48(H48), C41(H41), C34(H34), C52(H52)
5.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C28(H28A,H28B,H28C), C58(H58A,H58B,H58C), C30(H30A,H30B,
 H30C), C29(H29A,H29B,H29C), C28I(H28D,H28E,H28F), C29I(H29D,H29E,H29F),
 C30I(H30D,H30E,H30F), C58I(H58D,H58E,H58F)
;
_shelx_fab_checksum              13132
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'