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_4516979
_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         'C80 H78 N5 Si2 Y'
_chemical_formula_sum            'C80 H78 N5 Si2 Y'
_chemical_formula_weight         1254.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.137(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1287(7)
_cell_length_b                   22.4625(13)
_cell_length_c                   24.6736(14)
_cell_measurement_reflns_used    9389
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.22
_cell_measurement_theta_min      4.06
_cell_volume                     6722.1(7)
_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      100.02
_diffrn_detector                 'CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.69
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            114566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.873
_diffrn_reflns_theta_min         1.967
_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    1.925
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.5634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1325 before and 0.1131 after correction. The Ratio of minimum to maximum transmission is 0.7208. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         14399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+11.7172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13905
_reflns_number_total             14399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao9b01788_si_001.cif
_cod_data_source_block           DPPYInd2
_cod_database_code               4516979
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.831
_shelx_estimated_absorpt_t_min   0.699
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5946(8)
 0.4054(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C38(H38), C35(H35), C32(H32), C57(H57), C63(H63), C60(H60)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C50(H50), C44(H44), C4(H4), C46(H46), C13(H13), C12(H12), C45(H45),
 C52(H52), C66(H66), C18(H18), C5(H5), C43(H43), C26(H26), C8(H8), C28(H28),
 C20(H20), C25(H25), C51(H51), C21(H21), C14(H14), C53(H53), C3(H3), C19(H19),
 C78(H78), C67(H67), C70(H70), C27(H27), C71(H71), C77(H77), C74(H74), C69(H69),
  C79(H79), C75(H75), C72(H72), C80(H80)
3.c Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C40(H40A,H40B,H40C), C58(H58A,H58B,H58C), C36(H36A,H36B,
 H36C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C59(H59A,H59B,H59C), C34(H34A,
 H34B,H34C), C65(H65A,H65B,H65C), C33(H33A,H33B,H33C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C)
;
_shelx_res_checksum              97666
_shelx_hkl_checksum              3858
_olex2_submission_special_instructions 'No special instructions were received'