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_4089291
_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         'C31 H27 Cl3 Cr N P2, 2(C H2 Cl2)'
_chemical_formula_sum            'C33 H31 Cl7 Cr N P2'
_chemical_formula_weight         803.68
_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                75.733(6)
_cell_angle_beta                 81.438(5)
_cell_angle_gamma                73.265(5)
_cell_formula_units_Z            2
_cell_length_a                   10.8962(7)
_cell_length_b                   12.8113(15)
_cell_length_c                   13.8238(17)
_cell_measurement_reflns_used    1061
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.51
_cell_measurement_theta_min      2.52
_cell_volume                     1784.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3 v2016'
_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      100.02
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0544
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            112813
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_min         2.516
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.7069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.0711 before and 0.0553 after correction. 
The Ratio of minimum to maximum transmission is 0.9443. 
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.7486
_exptl_transmission_factor_min   0.7069
_refine_diff_density_max         1.142
_refine_diff_density_min         -1.250
_refine_diff_density_rms         0.088
_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     426
_refine_ls_number_reflns         17281
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+1.1625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13063
_reflns_number_total             17281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00189_si_003.cif
_cod_data_source_block           3
_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               4089291
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.824
_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. Restrained distances
 C34-Cl9 \\sim C34-Cl6
 with sigma of 0.02
 C33-Cl7 \\sim C33-Cl8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim Cl9 \\sim Cl6 \\sim C33 \\sim Cl7 \\sim Cl8: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(Cl9)=Sof(Cl6)=Sof(C34)=Sof(H34A)=Sof(H34B)=1-FVAR(1)
 Sof(Cl7)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(Cl8)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C19(H19), C13(H13), C23(H23), C12(H12), C3(H3), C18(H18),
 C28(H28), C27(H27), C21(H21), C5(H5), C31(H31), C17(H17), C10(H10), C25(H25),
 C16(H16), C6(H6), C11(H11), C22(H22), C15(H15), C24(H24), C30(H30), C29(H29)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              25228
_shelx_hkl_checksum              48355
_olex2_submission_special_instructions 'No special instructions were received'