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_4089292
_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         '0.5(C54 H54 Cl6 Cr2 N2 P4), 3(C H2 Cl2)'
_chemical_formula_sum            'C30 H33 Cl9 Cr N P2'
_chemical_formula_weight         840.56
_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     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                94.594(5)
_cell_angle_beta                 92.147(5)
_cell_angle_gamma                109.222(4)
_cell_formula_units_Z            4
_cell_length_a                   13.5833(11)
_cell_length_b                   14.3977(14)
_cell_length_c                   20.235(2)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.79
_cell_measurement_theta_min      2.66
_cell_volume                     3716.1(6)
_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      100.01
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            289169
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         40.000
_diffrn_reflns_theta_min         2.401
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.7479
_exptl_absorpt_correction_T_min  0.6318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0967 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.8448.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         44225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+4.3015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28611
_reflns_number_total             44225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00189_si_003.cif
_cod_data_source_block           4
_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_original_cell_volume        3716.2(6)
_cod_database_code               4089292
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H57C)=Sof(H57D)=Sof(Cl22)=Sof(Cl24)=1-FVAR(1)
 Sof(Cl23)=Sof(Cl21)=Sof(H57A)=Sof(H57B)=FVAR(1)
 Sof(H60C)=Sof(H60D)=Sof(Cl19)=Sof(Cl18)=1-FVAR(2)
 Sof(Cl20)=Sof(Cl17)=Sof(H60A)=Sof(H60B)=FVAR(2)
 Sof(H58C)=Sof(H58D)=Sof(Cl15)=1-FVAR(3)
 Sof(Cl16)=Sof(H58A)=Sof(H58B)=FVAR(3)
 Sof(H59C)=Sof(H59D)=Sof(Cl12)=1-FVAR(4)
 Sof(Cl13)=Sof(H59A)=Sof(H59B)=FVAR(4)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C57(H57C,H57D), C60(H60A,H60B), C60(H60C,H60D), C56(H56A,
 H56B), C58(H58A,H58B), C58(H58C,H58D), C59(H59A,H59B), C59(H59C,H59D),
 C55(H55A,H55B)
3.c Aromatic/amide H refined with riding coordinates:
 C54(H54), C25(H25), C15(H15), C17(H17), C13(H13), C11(H11), C50(H50),
 C47(H47), C7(H7), C14(H14), C23(H23), C27(H27), C24(H24), C48(H48), C42(H42),
 C32(H32), C52(H52), C6(H6), C53(H53), C5(H5), C34(H34), C33(H33), C51(H51),
 C12(H12), C9(H9), C39(H39), C40(H40), C36(H36), C26(H26), C19(H19), C21(H21),
 C45(H45), C41(H41), C44(H44), C46(H46), C38(H38), C35(H35), C8(H8), C20(H20),
 C18(H18)
3.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C29(H29A,H29B,H29C), C2(H2A,H2B,H2C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              27062
_shelx_hkl_checksum              20340
_olex2_submission_special_instructions 'No special instructions were received'