Unexpected Precatalyst σ-Ligand Effects in Phenoxyimine Zr-Catalyzed Ethylene/1-Octene Copolymerizations.
Gao, Yanshan; Christianson, Matthew D.; Wang, Yang; Chen, Jiazhen; Marshall, Steve; Klosin, Jerzy; Lohr, Tracy L.; Marks, Tobin J.; Journal of the American Chemical Society 141 (2019) 7822–7830; doi:10.1021/jacs.9b01445

data_4128223
_publ_section_title
;
 Unexpected Precatalyst \s-Ligand Effects in Phenoxyimine Zr-Catalyzed
 Ethylene/1-Octene Copolymerizations.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7822
_journal_page_last               7830
_journal_paper_doi               10.1021/jacs.9b01445
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C21 H36 Al N O, 0.5(C5 H12)'
_chemical_formula_sum            'C23.5 H42 Al N O'
_chemical_formula_weight         381.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.055(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2677(12)
_cell_length_b                   12.6644(8)
_cell_length_c                   19.5770(12)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.634
_cell_measurement_theta_min      4.135
_cell_volume                     4947.8(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14159
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        66.672
_diffrn_reflns_theta_max         66.672
_diffrn_reflns_theta_min         4.134
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0667 before and 0.0446 after correction. The Ratio of minimum to maximum transmission is 0.8674. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.024
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.256
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4265
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+6.3029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4140
_reflns_number_total             4265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01445_si_005.cif
_cod_data_source_block           cx1221
_cod_original_formula_sum        'C23.50 H42 Al N O'
_cod_database_code               4128223
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.756
_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. Rigid body (RIGU) restrains
 C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) C24(0.5) H24A(0.5) H24B(0.5) C25(0.5) H25A(0.5) H25B(0.5) C26(0.5)
 H26A(0.5) H26B(0.5) H26C(0.5)
4.a Ternary CH refined with riding coordinates:
 C19(H19)
4.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              78604
_shelx_hkl_checksum              29826
_olex2_date_sample_data_collection 2018-03-13
_olex2_date_sample_submission    2018-02-23
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx1221
_olex2_submission_special_instructions 'No special instructions were received'