Synthesis of Highly Branched Polyethylene Using “Sandwich” (8-p-Tolyl naphthyl α-diimine)nickel(II) Catalysts
Zhang, Danfeng; Nadres, Enrico T.; Brookhart, Maurice; Daugulis, Olafs; Organometallics 32 (2013) 5136–; doi:10.1021/om400704h

data_4081423
_publ_section_title
;
 Synthesis of Highly Branched Polyethylene Using &#x201C;Sandwich&#x201D;
 (8-p-Tolyl naphthyl \a-diimine)nickel(II) Catalysts
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5136
_journal_paper_doi               10.1021/om400704h
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C46 H32 Br2 N2 Ni, C H2 Cl2'
_chemical_formula_sum            'C47 H34 Br2 Cl2 N2 Ni'
_chemical_formula_weight         916.19
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-07-05
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2669(2)
_cell_length_b                   12.4336(2)
_cell_length_c                   13.9921(2)
_cell_measurement_reflns_used    5460
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.332
_cell_measurement_theta_min      3.55
_cell_volume                     1941.43(5)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_number            3427
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.572
_diffrn_reflns_theta_min         3.555
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.680
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.3235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0765 before and 0.0544 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0952 before and 0.0714 after correction.
 The Ratio of minimum to maximum transmission is 0.71.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 30028 reflections, Rint = 0.0691
 (11287 with I > 3sig(I), Rint = 0.0478)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+2.3105P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3016
_reflns_number_total             3427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400704h_si_002.cif
_cod_data_source_block           zdfb3
_cod_database_code               4081423
_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. Others
 Fixed Sof: H25A(0.5) H25B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C19(H19), C20(H20), C22(H22), C23(H23)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.405
_shelx_hkl_checksum              98019
_shelx_res_checksum              13664
_shelxl_version_number           2013-2