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_4516800
_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         'C30 H31 N O6 S'
_chemical_formula_sum            'C28 H25 N O5 S'
_chemical_formula_weight         487.55
_chemical_name_systematic        (SO2)-FI2-OMe2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2492(5)
_cell_length_b                   8.0522(2)
_cell_length_c                   31.5344(6)
_cell_measurement_reflns_used    9605
_cell_measurement_temperature    100
_cell_measurement_theta_max      64.98
_cell_measurement_theta_min      5.19
_cell_volume                     5141.7(2)
_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      100.04
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            47895
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.021
_diffrn_reflns_theta_max         65.021
_diffrn_reflns_theta_min         5.192
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0721 before and 0.0445 after correction. The Ratio of minimum to maximum transmission is 0.8626. 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    1.260
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2048
_exptl_crystal_preparation
'The compound is the dimethoxy-acetal of the half-substituted Fi2-SO2 moiety.'
_exptl_crystal_recrystallization_method
'The compound was crystallized from slow evaporation of a DCM-MeOH-toluene mixture at room temperature.'
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0378P)^2^+5.9808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4014
_reflns_number_total             4368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mz5b00781_si_005.cif
_cod_data_source_block           1am165_a
_cod_database_code               4516800
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.653
_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.a Ternary CH refined with riding coordinates:
 C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1A), C15(H15), C14(H14), C4(H4), C3(H3), C13(H13), C20(H20), C23(H23),
 C6(H6), C19(H19), C22(H22), C11(H11), C16(H16), C7(H7)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C25(H25A,H25B,
 H25C), C30(H30A,H30B,H30C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              70075
_shelx_hkl_checksum              63543
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method
'The crystal was mounted in Paratone-N on a brass tip.'
_olex2_submission_original_sample_id 1AM165
_olex2_submission_special_instructions 'No special instructions were received'