Chromium Aryl Complexes with N-Donor Ligands as Catalyst Precursors for Selective Ethylene Trimerization
Ronellenfitsch, Mathias; Wadepohl, Hubert; Enders, Markus; Organometallics 33 (2014) 5758–; doi:10.1021/om500459k

data_4084004
_publ_section_title
;
 Chromium Aryl Complexes with N-Donor Ligands as Catalyst Precursors
 for Selective Ethylene Trimerization
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5758
_journal_paper_doi               10.1021/om500459k
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C19 H27 Cl2 Cr N2 O, 0.5(C4 H8 O)'
_chemical_formula_sum            'C21 H31 Cl2 Cr N2 O1.5'
_chemical_formula_weight         458.38
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                en_mr22
_audit_creation_date
;
'Fri Dec 20 16:01:24 2013'
;
_audit_update_record             'Fri Apr 25 10:32:51 CEST 2014'
_cell_angle_alpha                94.5819(13)
_cell_angle_beta                 96.4707(14)
_cell_angle_gamma                107.7801(17)
_cell_formula_units_Z            4
_cell_length_a                   8.94124(16)
_cell_length_b                   13.0454(2)
_cell_length_c                   19.7127(3)
_cell_measurement_reflns_used    12032
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      30.4040
_cell_measurement_theta_min      3.5950
_cell_volume                     2159.62(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al., 2004)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -29.00   -1.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -78.0000  121.7386 56

  2 omega  -31.00   -5.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -79.0000   57.4253 52

  3 omega  -88.00  -62.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -77.0000 -150.0000 52

  4 omega  -36.00   -4.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -77.0000 -150.0000 64

  5 omega   -4.00   37.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502   57.0000   30.0000 82

  6 omega   58.00   97.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000  -30.0000 78

  7 omega   -1.00   25.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   79.0000   57.2943 52

  8 omega  -32.00    8.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -80.0000   77.5076 80

  9 omega   -1.00   24.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   79.0000   38.0872 50

 10 omega   14.00   44.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000   90.0000 60

 11 omega   12.00   60.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000    0.0000 96

 12 omega   71.00   99.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000    0.0000 56

 13 omega  -37.00   -7.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000    0.0000 60

 14 omega  -38.00   62.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000   30.0000 200

 15 omega  -38.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -80.0000  -58.1686 206

 16 omega    8.00   60.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   77.0000  -60.0000 104

 17 omega    0.00   32.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   77.0000  -90.0000 64

 18 omega    5.00   51.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   38.0000  -60.0000 92

 19 omega   12.00   90.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000  150.0000 156

 20 omega  -39.00   20.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -78.0000  121.7386 118

 21 omega   26.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -78.0000  121.7386 76

 22 omega    5.00   72.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   38.0000  120.0000 134

 23 omega  -27.00   45.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -38.0000 -180.0000 144

 24 omega   11.00   51.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000 -120.0000 80

 25 omega    7.00   46.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   38.0000  -30.0000 78

 26 omega  -27.00    7.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000 -180.0000 68

 27 omega   39.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000 -180.0000 50

 28 omega   21.00   63.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000  -30.0000 84

 29 omega   23.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -80.0000   77.5076 84

 30 omega   -2.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -79.0000 -139.8398 134

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0062053000
_diffrn_orient_matrix_UB_12      -0.0551872000
_diffrn_orient_matrix_UB_13      -0.0083516000
_diffrn_orient_matrix_UB_21      -0.0509675000
_diffrn_orient_matrix_UB_22      -0.0024557000
_diffrn_orient_matrix_UB_23      -0.0308074000
_diffrn_orient_matrix_UB_31      0.0667226000
_diffrn_orient_matrix_UB_32      0.0160279000
_diffrn_orient_matrix_UB_33      -0.0176616000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67531
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.526
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.1527
_exptl_crystal_size_mid          0.1010
_exptl_crystal_size_min          0.0699
_refine_diff_density_max         2.310
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         13183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.000
_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^+2.7386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9484
_reflns_number_total             13183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500459k_si_002.cif
_cod_data_source_block           en_mr22
_cod_original_formula_sum        'C21 H31 Cl2 Cr N2 O1.50'
_cod_database_code               4084004
_audit_block_refno               1938
_audit_block_usercomment         'mr231a, block, green'
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C21 H31 Cl2 Cr1 N2 O1.5'
_chemical_oxdiff_usercomment     'mr231a, block, green'
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.925
_reflns_odcompleteness_completeness 83.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.50
_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. Uiso/Uaniso restraints and constraints
C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim
C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim
C68 \\sim C69 \\sim C70 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7
\\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15
\\sim C16 \\sim C18 \\sim C19 \\sim C17 \\sim C20 \\sim C81 \\sim C82 \\sim C83
\\sim C84: within 1A with sigma of 0.01 and sigma for terminal atoms of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,
 H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C17(H17A,H17B), C81(H81A,
 H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
3.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C2(H2), C3(H3),
 C4(H4), C5(H5), C6(H6), C7(H7)
3.c Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              57026
_cell_oxdiff_length_a            8.94124(17)
_cell_oxdiff_length_b            13.0454(2)
_cell_oxdiff_length_c            19.7127(3)
_cell_oxdiff_angle_alpha         94.5819(13)
_cell_oxdiff_angle_beta          96.4707(14)
_cell_oxdiff_angle_gamma         107.7801(17)
_cell_oxdiff_volume              2159.63(6)
_cell_oxdiff_measurement_reflns_used 12032