Ligand-Unsymmetrical Phenoxyiminato Dinickel Catalyst for High Molecular Weight Long-Chain Branched Polyethylenes
Shu, Dongxu; Mouat, Aidan R.; Stephenson, Casey J.; Invergo, Anna M.; Delferro, Massimiliano; Marks, Tobin J.; ACS Macro Letters 4 (2015) 1297–; doi:10.1021/acsmacrolett.5b00781

data_4516803
_publ_section_title
;
 Ligand-Unsymmetrical Phenoxyiminato Dinickel Catalyst for High Molecular
 Weight Long-Chain Branched Polyethylenes
;
_journal_issue                   11
_journal_name_full               'ACS Macro Letters'
_journal_page_first              1297
_journal_paper_doi               10.1021/acsmacrolett.5b00781
_journal_volume                  4
_journal_year                    2015
_chemical_formula_moiety         'C52 H64 N2 Ni2 O6 P2 S2'
_chemical_formula_sum            'C52 H64 N2 Ni2 O6 P2 S2'
_chemical_formula_weight         1056.53
_chemical_name_systematic        Ni2-FI(SO2)
_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
_audit_creation_date             2015-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.487(2)
_cell_angle_beta                 98.374(2)
_cell_angle_gamma                107.462(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6834(4)
_cell_length_b                   14.3669(5)
_cell_length_c                   18.2980(5)
_cell_measurement_reflns_used    9521
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.07
_cell_measurement_theta_min      3.23
_cell_volume                     2894.18(17)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30397
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.213
_diffrn_reflns_theta_min         3.942
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.6438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0967 before and 0.0454 after correction.
The Ratio of minimum to maximum transmission is 0.8550.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         10365
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0737P)^2^+0.8366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1217
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8828
_reflns_number_total             10365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mz5b00781_si_002.cif
_cod_data_source_block           dxs_a
_cod_database_code               4516803
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.605
_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. Restrained distances
 C27-C24 \\sim C26-C24 \\sim C25-C24
 with sigma of 0.02
3. Others
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C31(H31), C4(H4), C22(H22), C36(H36), C40(H40), C28(H28), C30(H30),
 C39(H39), C20(H20), C19(H19), C23(H23), C13(H13), C3(H3), C33(H33), C10(H10),
 C32(H32), C11(H11), C9(H9), C14(H14), C15(H15), C37(H37)
4.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C25(H25A,H25B,H25C), C51(H51A,H51B,
 H51C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C48(H48A,H48B,H48C), C26(H26A,
 H26B,H26C), C25A(H25D,H25E,H25F), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C27(H27A,H27B,H27C), C26A(H26D,H26E,
 H26F), C27A(H27D,H27E,H27F), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              74077
_shelx_hkl_checksum              39574
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-06-10
_olex2_date_sample_submission    2015-06-10
_olex2_exptl_crystal_mounting_method
'The crystal was mounted under air-free conditions in Paratone-N on a brass tip.'
_olex2_submission_original_sample_id DXS_Ni2-FI(SO2)2
_olex2_submission_special_instructions 'No special instructions were received'