Ethylene Tetramerization Catalysis: Effects of Aluminum-Induced Isomerization of PNP to PPN Ligands
Lifschitz, Alejo M.; Hirscher, Nathanael A.; Lee, Heui Beom; Buss, Joshua A.; Agapie, Theodor; Organometallics 36 (2017) 1640–; doi:10.1021/acs.organomet.7b00189

data_4089296
_publ_section_title
;
 Ethylene Tetramerization Catalysis: Effects of Aluminum-Induced
 Isomerization of PNP to PPN Ligands
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1640
_journal_paper_doi               10.1021/acs.organomet.7b00189
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C24 H20 Al Cl3 O P2, C6 H6'
_chemical_formula_sum            'C30 H26 Al Cl3 O P2'
_chemical_formula_weight         597.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.913(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3545(11)
_cell_length_b                   9.3024(11)
_cell_length_c                   17.270(2)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.19
_cell_volume                     1470.5(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_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  0.0376
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61923
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.873
_diffrn_reflns_theta_min         2.189
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0728 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.9223.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 3863 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.485(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         9057
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0499P)^2^+0.1903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.981
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                8266
_reflns_number_total             9057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00189_si_003.cif
_cod_data_source_block           10
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4089296
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(Cl3)=Sof(Al2)=Sof(O2)=1-FVAR(1)
 Sof(Cl4)=Sof(Al1)=Sof(O1)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C16(H16), C6(H6), C15(H15), C18(H18), C2(H2), C17(H17), C8(H8),
 C12(H12), C14(H14), C9(H9), C20(H20), C10(H10), C22(H22), C3(H3), C24(H24),
 C23(H23), C26(H26), C5(H5), C30(H30), C4(H4), C25(H25), C27(H27), C29(H29),
 C28(H28), C21(H21)
;
_shelx_res_checksum              54469
_shelx_hkl_checksum              60434
_olex2_submission_special_instructions 'No special instructions were received'