Early Metal Di(pyridyl) Pyrrolide Complexes with Second Coordination Sphere Arene-π Interactions: Ligand Binding and Ethylene Polymerization.
Sampson, Jessica; Choi, Gyeongshin; Akhtar, Muhammed Naseem; Jaseer, E. A.; Theravalappil, Rajesh; Garcia, Nestor; Agapie, Theodor; ACS omega 4 (2019) 15879–15892; doi:10.1021/acsomega.9b01788

data_4516978
_publ_section_title
;
 Early Metal Di(pyridyl) Pyrrolide Complexes with Second Coordination
 Sphere Arene-\p Interactions: Ligand Binding and Ethylene Polymerization.
;
_journal_issue                   14
_journal_name_full               'ACS omega'
_journal_page_first              15879
_journal_page_last               15892
_journal_paper_doi               10.1021/acsomega.9b01788
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C76 H96 N3 O Si4 Y'
_chemical_formula_sum            'C76 H96 N3 O Si4 Y'
_chemical_formula_weight         1268.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                96.041(6)
_cell_angle_beta                 104.761(6)
_cell_angle_gamma                94.927(7)
_cell_formula_units_Z            2
_cell_length_a                   11.597(5)
_cell_length_b                   16.582(7)
_cell_length_c                   21.396(5)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.26
_cell_volume                     3929(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            117114
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         2.302
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0599 before and 0.0526 after correction. The Ratio of minimum to maximum transmission is 0.9524. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         18118
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+3.5831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14535
_reflns_number_total             18118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b01788_si_001.cif
_cod_data_source_block           DPPYr2THF
_cod_original_cell_volume        3930(2)
_cod_database_code               4516978
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.843
_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. Uiso/Uaniso restraints and constraints
C57: within 1.7A with sigma of 0.05 and sigma for terminal atoms of 0.1
C54 \\sim C55: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C54 \\sim C55A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
3. Rigid body (RIGU) restrains
 C54, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54, C55A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H54A)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C55)=Sof(H55A)=Sof(H55B)=
 Sof(H55C)=1-FVAR(1)
 Sof(H54)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C55A)=Sof(H55D)=Sof(H55E)=
 Sof(H55F)=FVAR(1)
 Sof(H57A)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(2)
 Sof(H57)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C57(H57A), C57(H57), C64(H64), C54(H54), C54(H54A), C32(H32), C27(H27),
 C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C72(H72A,H72B), C70(H70A,H70B), C68(H68A,H68B), C73(H73A,H73B), C71(H71A,
 H71B), C77(H77A,H77B)
5.c Aromatic/amide H refined with riding coordinates:
 C43(H43), C61(H61), C20(H20), C9(H9), C62(H62), C12(H12), C36(H36), C8(H8),
 C5(H5), C46(H46), C60(H60), C19(H19), C38(H38), C37(H37), C63(H63), C14(H14),
 C3(H3), C18(H18), C45(H45), C21(H21), C4(H4), C44(H44), C13(H13)
5.d Idealised Me refined as rotating group:
 C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C74(H74A,H74B,H74C), C78(H78A,H78B,
 H78C), C79(H79A,H79B,H79C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C80(H80A,H80B,H80C), C66(H66A,H66B,H66C), C26(H26A,H26B,H26C),
 C65(H65A,H65B,H65C), C31(H31A,H31B,H31C), C28(H28A,H28B,H28C), C53(H53A,H53B,
 H53C), C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C1AA(H1AA,H1AB,H1AC),
 C0AA(H0AA,H0AB,H0AC), C1(H1A,H1B,H1C), C55A(H55D,H55E,H55F)
;
_shelx_res_checksum              67487
_shelx_hkl_checksum              79479
_shelx_fab_checksum              93292
_olex2_submission_special_instructions 'No special instructions were received'