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_4516802
_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         'C50 H34 F12 N2 O4 S'
_chemical_formula_sum            'C50 H34 F12 N2 O4 S'
_chemical_formula_weight         986.85
_chemical_name_systematic        (CF3,SO2)FI-Ni2
_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     direct
_audit_creation_date             2015-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                86.808(2)
_cell_angle_beta                 78.729(2)
_cell_angle_gamma                74.8280(10)
_cell_formula_units_Z            2
_cell_length_a                   8.1727(3)
_cell_length_b                   15.1478(5)
_cell_length_c                   20.3994(7)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.10
_cell_measurement_theta_min      2.96
_cell_volume                     2390.35(15)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50832
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.135
_diffrn_reflns_theta_min         2.629
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0773 before and 0.0647 after correction.
The Ratio of minimum to maximum transmission is 0.9151.
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    1.371
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1008
_exptl_crystal_preparation
'The compound was prepared in refluxing DCM over molecular sieves.'
_exptl_crystal_recrystallization_method
'The compound was crystallized by slow evaporation of a dilute CDCl3 solution'
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.135
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         13636
_refine_ls_number_restraints     652
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0997
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1680P)^2^+1.7221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3008
_refine_ls_wR_factor_ref         0.3207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7844
_reflns_number_total             13636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mz5b00781_si_004.cif
_cod_data_source_block           1am207_a
_cod_database_code               4516802
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 F12-C33 \\sim F11-C33 \\sim F10-C33
 with sigma of 0.02
 C43-C42 \\sim C44-C43 \\sim C44-C45 \\sim C45-C46 \\sim C46-C41 \\sim C42-C41
 with sigma of 0.02
 C50-C47 \\sim C48-C47 \\sim C49-C47
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2A), C21(H21), C34(H34), C15(H15), C37(H37), C11(H11), C19(H19), C31(H31),
  C23(H23), C6(H6), C43(H43), C42(H42), C27(H27), C7(H7), C3AA(H3AA),
 C2AA(H2AA), C39(H39), C46(H46), C14(H14), C45(H45), C29(H29), C36(H36),
 C16(H16), C38(H38)
5.b Idealised Me refined as rotating group:
 C50(H50C,H50A,H50B), C49(H49B,H49A,H49C), C48(H48A,H48B,H48C)
5.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              98266
_shelx_hkl_checksum              68868
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method
'The compound was mounted in Paratone-N on a brass tip.'
_olex2_submission_original_sample_id 1AM207
_olex2_submission_special_instructions 'No special instructions were received'