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_4516977
_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         'C36 H40 Al N3'
_chemical_formula_sum            'C36 H40 Al N3'
_chemical_formula_weight         541.69
_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             2018-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                88.535(3)
_cell_angle_beta                 85.525(3)
_cell_angle_gamma                72.732(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0846(7)
_cell_length_b                   10.7246(7)
_cell_length_c                   14.7495(11)
_cell_measurement_reflns_used    5100
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.489
_cell_measurement_theta_min      2.421
_cell_volume                     1518.66(19)
_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      100.05
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1449
_diffrn_reflns_av_unetI/netI     0.0950
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21981
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_min         2.421
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0703 before and 0.0459 after correction. The Ratio of minimum to maximum transmission is 0.8915. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+0.6771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4480
_reflns_number_total             6355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b01788_si_001.cif
_cod_data_source_block           DPPAlEt2
_cod_database_code               4516977
_shelx_shelxl_version_number     2017/1
_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.a Secondary CH2 refined with riding coordinates:
 C36(H00E,H00F), C34(H00H,H00L)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H006), C8(H008), C5(H00A), C22(H00G), C4(H00I), C28(H00J), C12(H00K),
 C19(H00P), C13(H00V), C3(H00X), C14(H00Y), C31(H00Z)
2.c Idealised Me refined as rotating group:
 C18(H00B,H00C,H00D), C37(H00M,H00N,H00O), C27(H00Q,H00R,H00S), C35(H01A,H01B,
 H01C), C24(H01D,H01E,H01F), C30(H01G,H01H,H01I), C21(H01J,H01K,H01L), C33(H01M,
 H01N,H01O)
;
_shelx_res_checksum              65283
_shelx_hkl_checksum              27687
_olex2_submission_special_instructions 'No special instructions were received'