Polar Additive Triggered Branching Switch and Block Polyolefin Topology in Living Ethylene Polymerization
Zhang, Yuxing; Jian, Zhongbao; Macromolecules  (2021) –; doi:10.1021/acs.macromol.1c00174

data_1561043
_publ_section_title
;
 Polar Additive Triggered Branching Switch and Block Polyolefin Topology
 in Living Ethylene Polymerization
;
_journal_name_full               Macromolecules
_journal_paper_doi               10.1021/acs.macromol.1c00174
_journal_year                    2021
_chemical_formula_moiety         'C90 H62 N3 O2 Pd, C32 H12 B F24'
_chemical_formula_sum            'C122 H74 B F24 N3 O2 Pd'
_chemical_formula_weight         2187.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                82.810(2)
_cell_angle_beta                 78.691(2)
_cell_angle_gamma                86.591(2)
_cell_formula_units_Z            2
_cell_length_a                   17.8161(11)
_cell_length_b                   17.9108(10)
_cell_length_c                   19.3137(10)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    206(2)
_cell_measurement_theta_max      27.823
_cell_measurement_theta_min      2.293
_cell_volume                     5992.0(6)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      206.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'bruker apex ccd'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1167
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            235668
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.964
_diffrn_reflns_theta_min         2.126
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.348
_refine_diff_density_min         -1.576
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1391
_refine_ls_number_reflns         28657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1057P)^2^+11.2225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22595
_reflns_number_total             28657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma1c00174_si_002.cif
_cod_data_source_block           mo_20201102001_0m_sq
_cod_database_code               1561043
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.927
_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. Others
 Sof(H3B)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=1-FVAR(1)
 Sof(H3A)=Sof(C4)=Sof(H4A)=Sof(H4B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C00Y(H00Y), C010(H010), C017(H017), C01C(H01C), C01X(H01X), C01Y(H01Y),
 C020(H020), C024(H024), C02C(H02C), C02D(H02D)
3.b Aromatic/amide H refined with riding coordinates:
 C00Z(H00Z), C016(H016), C01A(H01A), C01D(H01D), C01K(H01K), C01L(H01L),
 C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R), C01V(H01V),
 C01W(H01W), C021(H021), C02E(H02E), C02G(H02G), C02J(H02J), C02K(H02K),
 C02M(H02M), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R), C02S(H02S),
 C02V(H02V), C02W(H02W), C02X(H02X), C032(H032), C033(H033), C034(H034),
 C036(H036), C038(H038), C03A(H03D), C03C(H03E), C03E(H03F), C03F(H03G),
 C03H(H03H), C03J(H03J), C03L(H03L), C03M(H03M), C03P(H03P), C03Q(H03Q),
 C03R(H03R), C03S(H03S), C03T(H03T), C03U(H03U), C03V(H03V), C03X(H03X),
 C042(H042), C044(H044), C048(H048), C04B(H04D), C3(H3A), C3(H3B)
3.c X=CH2 refined with riding coordinates:
 C4(H4A,H4B), C4A(H4AA,H4AB)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C037(H03A,H03B,H03C), C043(H04A,H04B,H04C)
;
_shelx_res_checksum              92426
_shelx_hkl_checksum              88822
_shelx_fab_checksum              91987
_olex2_submission_special_instructions 'No special instructions were received'