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_1547494
_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         'C56 H48 Br2 N2 Ni'
_chemical_formula_sum            'C56 H48 Br2 N2 Ni'
_chemical_formula_weight         967.45
_chemical_name_systematic
;
 ? 
;
_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_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-06-01 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.777(3)
_cell_length_b                   19.699(4)
_cell_length_c                   18.981(4)
_cell_measurement_reflns_used    15274
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4817
_cell_measurement_theta_min      1.1200
_cell_volume                     4579.5(19)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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: 270.0000
                 XTD: 39.9859
              2theta: -20.1645
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: 90.0000
                 XTD: 39.9859
              2theta: -20.1645
scan:
    Number of images: 328
               Slice: -110.0000 - 54.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 39.9859
              2theta: -20.1645
;
_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_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0645
_diffrn_orient_matrix_UB_12      0.0071
_diffrn_orient_matrix_UB_13      -0.0496
_diffrn_orient_matrix_UB_21      -0.0028
_diffrn_orient_matrix_UB_22      -0.0505
_diffrn_orient_matrix_UB_23      -0.0036
_diffrn_orient_matrix_UB_31      -0.0446
_diffrn_orient_matrix_UB_32      0.0001
_diffrn_orient_matrix_UB_33      0.0322
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59049
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.96
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.208
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7354
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1984.0
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.128
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         10500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+4.0075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                10006
_reflns_number_total             10500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7py01606a2.cif
_cod_data_source_block           Ni1
_cod_database_code               1547494
_diffrn_number_total             10824
_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:
 C31(H31), C44(H44)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C23(H23), C50(H50), C10(H10), C25(H25), C40(H40), C42(H42), C3(H3),
 C46(H46), C39(H39), C9(H9), C8(H8), C53(H53), C37(H37), C47(H47), C56(H56),
 C33(H33), C43(H43), C54(H54), C49(H49), C52(H52), C4(H4), C15(H15), C17(H17),
 C55(H55), C36(H36), C35(H35), C41(H41), C34(H34), C16(H16), C48(H48)
2.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'