Role of Radical Species in Salicylaldiminato Ni(II) Mediated Polymer Chain Growth: A Case Study for the Migratory Insertion Polymerization of Ethylene in the Presence of Methyl Methacrylate.
Ölscher, Franz; Göttker-Schnetmann, Inigo; Monteil, Vincent; Mecking, Stefan; Journal of the American Chemical Society 137 (2015) 14819–14828; doi:10.1021/jacs.5b08612

data_4129599
_publ_section_title
;
 Role of Radical Species in Salicylaldiminato Ni(II) Mediated Polymer
 Chain Growth: A Case Study for the Migratory Insertion Polymerization of
 Ethylene in the Presence of Methyl Methacrylate.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14819
_journal_page_last               14828
_journal_paper_doi               10.1021/jacs.5b08612
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C43 H40 I2 N Ni O P'
_chemical_formula_sum            'C43 H40 I2 N Ni O P'
_chemical_formula_weight         930.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.11 svn.r2872 for OlexSys, GUI svn.r4767)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.384(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7972(4)
_cell_length_b                   28.2682(8)
_cell_length_c                   13.0939(4)
_cell_measurement_reflns_used    77109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.59
_cell_volume                     4308.2(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED32'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            62211
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.875
_diffrn_reflns_theta_min         2.593
_exptl_absorpt_coefficient_mu    1.951
_exptl_absorpt_correction_T_max  0.4557
_exptl_absorpt_correction_T_min  0.2813
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         9141
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+3.3195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8325
_reflns_number_total             9141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b08612_si_002.cif
_cod_data_source_block           \fo14_131_s
_cod_database_code               4129599
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C44(H44), C45(H45)
2.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C52(H52), C51(H51), C10(H10), C11(H11), C12(H12), C50(H50),
 C48(H48), C49(H49), C56(H56), C57(H57), C27(H27), C28(H28), C29(H29), C54(H54),
  C55(H55), C33(H33), C34(H34), C35(H35), C36(H36), C47(H47), C39(H39),
 C40(H40), C41(H41), C42(H42), C46(H46)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              7036
_shelx_hkl_checksum              8220
_shelx_fab_checksum              4135
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'