Highly Robust Nickel Catalysts Containing Anilinonaphthoquinone Ligand for Copolymerization of Ethylene and Polar Monomers
Fu, Xia; Zhang, Lingjun; Tanaka, Ryo; Shiono, Takeshi; Cai, Zhengguo; Macromolecules 50 (2017) 9216–; doi:10.1021/acs.macromol.7b01947

data_1548123
_publ_section_title
;
 Highly Robust Nickel Catalysts Containing Anilinonaphthoquinone Ligand
 for Copolymerization of Ethylene and Polar Monomers
;
_journal_issue                   23
_journal_name_full               Macromolecules
_journal_page_first              9216
_journal_paper_doi               10.1021/acs.macromol.7b01947
_journal_volume                  50
_journal_year                    2017
_chemical_formula_moiety         'C67 H52 N Ni O2 P, 0.5(C4 H8 O)'
_chemical_formula_sum            'C69 H56 N Ni O2.5 P'
_chemical_formula_weight         1028.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                70.348(5)
_cell_angle_beta                 89.603(6)
_cell_angle_gamma                82.381(6)
_cell_formula_units_Z            4
_cell_length_a                   14.357(4)
_cell_length_b                   19.656(6)
_cell_length_c                   20.951(6)
_cell_measurement_reflns_used    2354
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22.57
_cell_measurement_theta_min      2.39
_cell_volume                     5514(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.2311
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25171
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         1.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0916 before and 0.0568 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1198 before and 0.0699 after correction.
 The Ratio of minimum to maximum transmission is 0.53.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 59976 reflections, Rint = 0.1019
 (13889 with I > 3sig(I), Rint = 0.0680)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.707
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1344
_refine_ls_number_reflns         25152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1939
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1213P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10905
_reflns_number_total             25152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma7b01947_si_002.cif
_cod_data_source_block           dm16887
_cod_depositor_comments
'Adding full bibliography for 1548123--1548124.cif.'
_cod_original_formula_sum        'C69 H56 N Ni O2.50 P'
_cod_database_code               1548123
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.882
_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.a Ternary CH refined with riding coordinates:
 C90(H90), C104(H104), C23(H23), C37(H37)
2.b Secondary CH2 refined with riding coordinates:
 C135(H13G,H13H), C136(H13A,H13B), C137(H13C,H13D), C138(H13E,H13F)
2.c Aromatic/amide H refined with riding coordinates:
 C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C76(H76), C77(H77),
 C78(H78), C79(H79), C82(H82), C86(H86), C88(H88), C92(H92), C93(H93), C94(H94),
  C95(H95), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102),
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C112(H112),
 C113(H113), C114(H114), C115(H115), C116(H116), C118(H118), C119(H119),
 C120(H120), C121(H121), C122(H122), C124(H124), C125(H125), C126(H126),
 C127(H127), C128(H128), C130(H130), C131(H131), C132(H132), C133(H133),
 C134(H134), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11),
  C12(H12), C15(H15), C19(H19), C21(H21), C25(H25), C26(H26), C27(H27),
 C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C39(H39),
  C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47),
 C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C57(H57),
  C58(H58), C59(H59), C60(H60), C61(H61), C63(H63), C64(H64), C65(H65),
 C66(H66), C67(H67)
2.d Idealised Me refined as rotating group:
 C103(H10A,H10B,H10C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              35291
_shelx_hkl_checksum              56703
_shelx_fab_checksum              83855
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'