Synthesis of Branched Polyethylene with “Half-Sandwich” Pyridine-Imine Nickel Complexes
Chen, Zhou; Allen, Kate E.; White, Peter S.; Daugulis, Olafs; Brookhart, Maurice; Organometallics 35 (2016) 1756–; doi:10.1021/acs.organomet.6b00165

data_4088534
_publ_section_title
;
 Synthesis of Branched Polyethylene with &#x201C;Half-Sandwich&#x201D;
 Pyridine-Imine Nickel Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1756
_journal_paper_doi               10.1021/acs.organomet.6b00165
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C50 H44 Br4 N4 Ni2, 2(C3 H6 O)'
_chemical_formula_sum            'C56 H56 Br4 N4 Ni2 O2'
_chemical_formula_weight         1254.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                96.9349(16)
_cell_angle_beta                 97.0991(17)
_cell_angle_gamma                107.7220(16)
_cell_formula_units_Z            1
_cell_length_a                   9.5363(4)
_cell_length_b                   10.2016(4)
_cell_length_c                   14.0506(6)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.03
_cell_measurement_theta_min      3.22
_cell_volume                     1273.81(9)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24149
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.061
_diffrn_reflns_theta_min         3.215
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.953
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.5742
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0470 before and 0.0383 after correction.
The Ratio of minimum to maximum transmission is 0.7651.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.8683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4478
_reflns_number_total             4712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00165_si_001.cif
_cod_data_source_block           x1509004
_cod_database_code               4088534
_shelx_estimated_absorpt_t_max   0.678
_shelx_estimated_absorpt_t_min   0.495
_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 Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C18(H18),
 C19(H19), C20(H20), C23(H23), C26(H26), C29(H29)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              90673
_shelx_hkl_checksum              45770
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'