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_4516976
_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         'C50 H54 N5 Si4 Y, 0.5(C6 H6)'
_chemical_formula_sum            'C53 H57 N5 Si4 Y'
_chemical_formula_weight         965.30
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                66.153(4)
_cell_angle_beta                 86.673(4)
_cell_angle_gamma                89.451(4)
_cell_formula_units_Z            4
_cell_length_a                   12.8334(15)
_cell_length_b                   18.935(2)
_cell_length_c                   21.972(2)
_cell_measurement_reflns_used    5784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.647
_cell_measurement_theta_min      2.353
_cell_volume                     4874.6(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.976
_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_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23285
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         1.015
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 150742 reflections, Rint = 0.0585
 (46063 with I > 3sig(I), Rint = 0.0309)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1271
_refine_ls_number_reflns         23285
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0668P)^2^+3.3620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17452
_reflns_number_total             23285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b01788_si_001.cif
_cod_data_source_block           DPPYTMDS2
_cod_original_cell_volume        4874.6(10)
_cod_database_code               4516976
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.805
_shelx_estimated_absorpt_t_min   0.698
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7344(7)
 0.2656(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
N4A \\sim Si4A \\sim Si5A \\sim C51A \\sim C50A: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A \\sim C21A \\sim C22A \\sim
C23A \\sim C24A \\sim C29A \\sim C28A \\sim C27A \\sim C26A \\sim C25A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C50A, Si5A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Si1B)=Sof(H1B)=Sof(C45B)=Sof(H45a)=Sof(H45b)=Sof(H45c)=Sof(Si4B)=
 Sof(H4Ba)=Sof(C49B)=Sof(H49a)=Sof(H49b)=Sof(H49c)=Sof(C48B)=Sof(H48a)=
 Sof(H48b)=Sof(H48c)=Sof(C44B)=Sof(H44a)=Sof(H44b)=Sof(H44c)=1-FVAR(1)
 Sof(C51B)=Sof(H51a)=Sof(H51b)=Sof(H51c)=Sof(Si3B)=Sof(H3Ba)=Sof(C47B)=
 Sof(H47a)=Sof(H47b)=Sof(H47c)=Sof(Si2B)=Sof(H2B)=Sof(C50B)=Sof(H50a)=Sof(H50b)=
 Sof(H50c)=Sof(C46B)=Sof(H46a)=Sof(H46b)=Sof(H46c)=FVAR(1)
 Sof(H51g)=Sof(H51h)=Sof(H51i)=Sof(Si5A)=Sof(H5Aa)=Sof(C50A)=Sof(H50d)=
 Sof(H50e)=Sof(H50f)=1-FVAR(2)
 Sof(Si4A)=Sof(H4Aa)=Sof(C49A)=Sof(H49d)=Sof(H49e)=Sof(H49f)=Sof(H51d)=
 Sof(H51e)=Sof(H51f)=FVAR(2)
 Sof(H52d)=Sof(H52e)=Sof(H52f)=Sof(C54B)=Sof(H54a)=Sof(H54b)=Sof(H54c)=
 Sof(Si6B)=Sof(H6B)=1-FVAR(3)
 Sof(H52a)=Sof(H52b)=Sof(H52c)=Sof(C53B)=Sof(H53a)=Sof(H53b)=Sof(H53c)=
 Sof(Si5B)=Sof(H5Ba)=FVAR(3)
 Sof(H55d)=Sof(H55e)=Sof(H55f)=Sof(C57B)=Sof(H57a)=Sof(H57b)=Sof(H57c)=
 Sof(Si8B)=Sof(H8B)=1-FVAR(4)
 Sof(H55a)=Sof(H55b)=Sof(H55c)=Sof(C58B)=Sof(H58a)=Sof(H58b)=Sof(H58c)=
 Sof(Si7B)=Sof(H7B)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 Si2A(H2A), Si3A(H3A), Si1A(H1A), Si3B(H3Ba), Si1B(H1B), Si2B(H2B), Si4B(H4Ba),
  Si4A(H4Aa), Si5A(H5Aa), Si7B(H7B), Si8B(H8B), Si6B(H6B), Si5B(H5Ba)
6.b Aromatic/amide H refined with riding coordinates:
 C23B(H23B), C12B(H12B), C13B(H13B), C32B(H32B), C3A(H3Aa), C18B(H18B),
 C28B(H28B), C32A(H32A), C37A(H37A), C4A(H4A), C9A(H9A), C8A(H8A), C4B(H4B),
 C5B(H5B), C3B(H3B), C9B(H9B), C21B(H21B), C56B(H56B), C20B(H20B), C5A(H5A),
 C19B(H19B), C25B(H25B), C33B(H33B), C14B(H14B), C42A(H42A), C37B(H37B),
 C42B(H42B), C35B(H35B), C39A(H39A), C14A(H14A), C39B(H39B), C12A(H12A),
 C34B(H34B), C33A(H33A), C27B(H27B), C13A(H13A), C35A(H35A), C40B(H40B),
 C26B(H26B), C41B(H41B), C41A(H41A), C25A(H25A), C40A(H40A), C34A(H34A),
 C61(H61), C60(H60), C62(H62), C64(H64), C63(H63), C65(H65), C21A(H21A),
 C19A(H19A), C18A(H18A), C23A(H23A), C20A(H20A), C26A(H26A), C27A(H27A),
 C28A(H28A)
6.c Idealised Me refined as rotating group:
 C46A(H46d,H46e,H46f), C48A(H48d,H48e,H48f), C45A(H45d,H45e,H45f), C52A(H52g,
 H52h,H52i), C47A(H47d,H47e,H47f), C44A(H44d,H44e,H44f), C51B(H51a,H51b,H51c),
 C47B(H47a,H47b,H47c), C45B(H45a,H45b,H45c), C49B(H49a,H49b,H49c), C50B(H50a,
 H50b,H50c), C48B(H48a,H48b,H48c), C46B(H46a,H46b,H46c), C44B(H44a,H44b,H44c),
 C49A(H49d,H49e,H49f), C51A(H51d,H51e,H51f), C51A(H51g,H51h,H51i), C52B(H52d,
 H52e,H52f), C52B(H52a,H52b,H52c), C55B(H55a,H55b,H55c), C55B(H55d,H55e,H55f),
 C57B(H57a,H57b,H57c), C50A(H50d,H50e,H50f), C58B(H58a,H58b,H58c), C53B(H53a,
 H53b,H53c), C54B(H54a,H54b,H54c)
;
_shelx_res_checksum              53122
_shelx_hkl_checksum              76789
_olex2_submission_special_instructions 'No special instructions were received'