Macrocyclic Trinuclear Nickel Phenoxyimine Catalysts for High-Temperature Polymerization of Ethylene and Isospecific Polymerization of Propylene
Chen, Zhongtao; Zhao, Xiangxiang; Gong, Xinyi; Xu, Di; Ma, Yuguo; Macromolecules 50 (2017) 6561–; doi:10.1021/acs.macromol.7b00996

data_1547542
_publ_section_title
;
 Macrocyclic Trinuclear Nickel Phenoxyimine Catalysts for High-Temperature
 Polymerization of Ethylene and Isospecific Polymerization of Propylene
;
_journal_issue                   17
_journal_name_full               Macromolecules
_journal_page_first              6561
_journal_paper_doi               10.1021/acs.macromol.7b00996
_journal_volume                  50
_journal_year                    2017
_chemical_formula_moiety         'C105 H105 N3 O6, 0.5(C6 H12)'
_chemical_formula_sum            'C108 H111 N3 O6'
_chemical_formula_weight         1546.99
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   20.4648(8)
_cell_length_b                   20.4648(8)
_cell_length_c                   73.392(3)
_cell_measurement_reflns_used    7318
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      26.4350
_cell_measurement_theta_min      3.1830
_cell_volume                     26619.2(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega   36.50  101.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  178.0000  -60.0000 86

  2 omega  -51.00   22.50   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -38.0000   60.0000 98

  3 omega  -55.00   -7.00   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -54.0000  144.0000 64

  4 omega   -8.00   29.50   0.7500   18.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.7954  -99.0000   60.0000 50
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0338654000
_diffrn_orient_matrix_UB_12      0.0353815000
_diffrn_orient_matrix_UB_13      0.0000232000
_diffrn_orient_matrix_UB_21      -0.0095939333
_diffrn_orient_matrix_UB_22      0.0085472333
_diffrn_orient_matrix_UB_23      -0.0086148667
_diffrn_orient_matrix_UB_31      -0.0190179333
_diffrn_orient_matrix_UB_32      0.0166337333
_diffrn_orient_matrix_UB_33      0.0043809333
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1372
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       87
_diffrn_reflns_limit_l_min       -90
_diffrn_reflns_number            44798
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.054
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             9936
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5790
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1122P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1909
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2808
_reflns_number_total             5790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma7b00996_si_003.cif
_cod_data_source_block           exp_6916
_cod_depositor_comments
;

2019-04-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        26619(2)
_cod_original_formula_moiety     '2(C105 H105 N3 O6), C6 H12'
_cod_original_formula_sum        'C216 H222 N6 O12'
_cod_original_formula_units_Z    6
_cod_original_formula_weight     3093.98
_cod_database_code               1547542
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C1H1O1
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.993
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.008
Uanis(C36) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.2
3.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18),
 C20(H20), C24(H24), C31(H31)
3.d Tetrahedral OH refined with riding coordinates:
 O2(H2)
3.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C35(H35A,H35B,H35C)
;
_olex2_submission_special_instructions 'No special instructions were received'