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_4089297
_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
'C64 H60 Cl3 Cr2 N2 P4, 0.5(C0.77 H2.3 Al Cl3.23), 0.5(C0.69 H2.06 Al Cl3.31), 2(C7 H8)'
_chemical_formula_sum            'C78.76 H78.28 Al Cl6.24 Cr2 N2 P4'
_chemical_formula_weight         1528.95
_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                68.6350(10)
_cell_angle_beta                 88.7120(10)
_cell_angle_gamma                88.3820(10)
_cell_formula_units_Z            4
_cell_length_a                   14.6582(5)
_cell_length_b                   22.7883(8)
_cell_length_c                   24.5404(9)
_cell_measurement_reflns_used    9636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.44
_cell_measurement_theta_min      2.48
_cell_volume                     7630.3(5)
_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 10.24
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            215976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.499
_diffrn_reflns_theta_min         2.240
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0795 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.9317.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_meas      ?
_exptl_crystal_description       slab
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1727
_refine_ls_number_reflns         46404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0572
_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^)+(0.0409P)^2^+14.9482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32344
_reflns_number_total             46404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00189_si_003.cif
_cod_data_source_block           11
_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               4089297
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.882
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=1-FVAR(1)
 Sof(Cl00)=FVAR(1)
 Sof(C)=Sof(HA)=Sof(HB)=Sof(HC)=1-FVAR(2)
 Sof(Cl01)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C011(H011), C012(H012), C018(H018), C019(H019), C01B(H01B),
 C01D(H01K), C01G(H01G), C01I(H01I), C01J(H01J), C01M(H01M), C01N(H01N),
 C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T),
 C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y), C021(H021),
 C023(H023), C025(H025), C026(H026), C027(H027), C028(H028), C02A(H02E),
 C02B(H02G), C02C(H02C), C02D(H02H), C02E(H02I), C02F(H02F), C02G(H02J),
 C02I(H02L), C02K(H02K), C02L(H02M), C02O(H02O), C02P(H02P), C02Q(H02Q),
 C02S(H02S), C02T(H02T), C02U(H02U), C02V(H02V), C02W(H02W), C02X(H02X),
 C02Y(H02Y), C02Z(H02Z), C031(H031), C032(H032), C033(H033), C034(H034),
 C035(H035), C036(H036), C037(H037), C038(H038), C039(H039), C03A(H03D),
 C03B(H03F), C03C(H03), C03E(H03E), C03F(H03I), C03G(H03G), C03H(H03H),
 C03I(H03K), C03J(H03J), C03M(H03M), C03N(H03T), C03O(H0AA), C03P(H03P),
 C03Q(H03Q), C03R(H03R), C03S(H03S), C03T(H03U), C03U(H03V), C03V(H03X),
 C03W(H03W), C03X(H03Y), C03Y(H03Z), C03Z(H1AA), C040(H040), C041(H041),
 C042(H042), C043(H043), C044(H044), C045(H045), C046(H046), C048(H048),
 C049(H049), C04B(H04E), C04C(H04C), C04D(H04F), C04E(H04O), C04G(H04G),
 C04H(H04H), C04I(H04L), C04K(H04M), C04L(H04V), C04N(H04N), C04O(H04),
 C04P(H2AA), C04Q(H04Q), C04S(H04W), C04T(H04T), C04U(H04U), C04V(H3AA),
 C04X(H04X), C04Y(H04Y), C04Z(H04Z), C050(H050), C051(H051), C053(H053),
 C054(H054), C055(H055)
5.b Idealised Me refined as rotating group:
 C01A(H01E,H01F,H01H), C01F(H01A,H01C,H01D), C02N(H02A,H02B,H02D), C03D(H03A,
 H03B,H03C), C03L(H03L,H03N,H03O), C04F(H04I,H04J,H04K), C04M(H04P,H04R,H04S),
 C04R(H04A,H04B,H04D), C052(H05D,H05E,H05F), C056(H05J,H05K,H05L), C057(H05G,
 H05H,H05I), C058(H05A,H05B,H05C), C0AA(H0AB,H0AC,H0AD), C(HA,HB,HC)
;
_shelx_res_checksum              75059
_shelx_hkl_checksum              85694
_olex2_submission_special_instructions 'No special instructions were received'