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_4516981
_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         'C38 H48 N6 Ti'
_chemical_formula_sum            'C38 H48 N6 Ti'
_chemical_formula_weight         636.72
_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             2019-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                73.736(3)
_cell_angle_beta                 87.627(3)
_cell_angle_gamma                88.402(3)
_cell_formula_units_Z            4
_cell_length_a                   13.9945(10)
_cell_length_b                   14.8672(11)
_cell_length_c                   17.6684(12)
_cell_measurement_reflns_used    9189
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.460
_cell_measurement_theta_min      2.403
_cell_volume                     3525.4(4)
_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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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  0.0956
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            311030
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         2.200
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0654 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.9702. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       wedge
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         16185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0477P)^2^+1.5088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13455
_reflns_number_total             16185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b01788_si_001.cif
_cod_data_source_block           DPPTiNMe2
_cod_database_code               4516981
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12B(H00F), C9B(H00I), C8B(H00O), C8A(H00T), C12A(H00U), C9A(H00W),
 C14B(H00X), C13B(H014), C22B(H015), C5B(H017), C32B(H01F), C29B(H01H),
 C14A(H01), C31A(H0AA), C19A(H1AA), C13A(H2AA), C19B(H01Q), C22A(H3AA),
 C4A(H4AA), C28A(H5AA), C3B(H020), C5A(H021), C3A(H023), C4B(H024)
2.b Idealised Me refined as rotating group:
 C28B(H01A,H01B,H01C), C39B(H01D,H01E,H01G), C38B(H01I,H01J,H01K), C34B(H01L,
 H01M,H01N), C25B(H24B,H01P,H01R), C18B(H01S,H01T,H01U), C37B(H01V,H01W,H01X),
 C40B(H01Y,H,HA), C36B(H01Z,HB,HC), C34A(H02J,H02K,H02L), C37A(H02M,H02N,H02O),
 C24A(H02P,H02Q,H02R), C18A(H02S,H02T,H02U), C35B(H02A,H02B,H02C), C36A(H02V,
 H02W,H02X), C39A(H02Y,HD,HE), C21A(H02Z,HF,HG), C35A(H02,HH,HI), C33A(H6AA,HJ,
 HK), C38A(H7AA,HL,HM), C31B(H02D,H02E,H02F), C30A(H8AA,HN,HO), C27A(H9AA,HP,
 HQ), C21B(H02G,H02H,H02I)
;
_shelx_res_checksum              42601
_shelx_hkl_checksum              43785
_olex2_submission_special_instructions 'No special instructions were received'