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_4084002
_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         'C24 H27 Cl2 Cr N2 O'
_chemical_formula_sum            'C24 H27 Cl2 Cr N2 O'
_chemical_formula_weight         482.37
_chemical_properties_physical    moisture-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     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                en_mr16
_audit_creation_date
;
'Fri Sep 27 11:31:31 2013'
;
_audit_update_record             'Fri Apr 25 10:37:53 CEST 2014'
_cell_angle_alpha                77.991(3)
_cell_angle_beta                 75.246(3)
_cell_angle_gamma                75.627(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3916(3)
_cell_length_b                   11.1195(3)
_cell_length_c                   12.5963(4)
_cell_measurement_reflns_used    13957
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      33.6300
_cell_measurement_theta_min      3.6120
_cell_volume                     1087.79(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
  1 omega   -9.00   18.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2064 -112.0000  -92.0357 54

  2 omega   -7.00   19.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2064 -113.0000   52.8584 52

  3 omega  -88.00  -33.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2064  121.0000   34.0000 110

  4 omega  -13.00   76.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -99.0000 -150.0000 178

  5 omega   11.00   58.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   57.0000 -180.0000 94

  6 omega   11.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   57.0000 -120.0000 180

  7 omega  -31.00   52.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -38.0000  -30.0000 166

  8 omega   16.00  105.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   38.0000  150.0000 178

  9 omega    1.00   84.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   77.0000   30.0000 166

 10 omega    5.00  104.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   38.0000    0.0000 198

 11 omega  -37.00   45.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -57.0000   90.0000 164

 12 omega   76.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   57.0000 -180.0000 50

 13 omega   41.00  110.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  178.0000   30.0000 138

 14 omega  -42.00   44.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -19.0000 -180.0000 172

 15 omega  -40.00   60.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -38.0000 -120.0000 200

 16 omega   11.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   57.0000  -30.0000 180

 17 omega   11.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   57.0000  150.0000 180

 18 omega  -37.00   54.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -57.0000 -180.0000 182

 19 omega  -40.00   19.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -38.0000    0.0000 118

 20 omega   55.00  103.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  154.0000 -167.0000 96

;
_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      -0.0144203000
_diffrn_orient_matrix_UB_12      -0.0004923000
_diffrn_orient_matrix_UB_13      0.0580593000
_diffrn_orient_matrix_UB_21      0.0768771000
_diffrn_orient_matrix_UB_22      0.0196663000
_diffrn_orient_matrix_UB_23      -0.0075738000
_diffrn_orient_matrix_UB_31      -0.0431514000
_diffrn_orient_matrix_UB_32      0.0636823000
_diffrn_orient_matrix_UB_33      -0.0067508000
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42413
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.101
_diffrn_reflns_theta_min         3.363
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       needle
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.3463
_exptl_crystal_size_mid          0.0856
_exptl_crystal_size_min          0.0594
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         8572
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0345P)^2^+0.6038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7014
_reflns_number_total             8572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500459k_si_002.cif
_cod_data_source_block           en_mr16
_cod_original_cell_volume        1087.79(7)
_cod_database_code               4084002
_audit_block_refno               1859
_audit_block_usercomment         'mr153c, needle, red'
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C24 H27 Cl2 Cr N2 O'
_chemical_oxdiff_usercomment     'mr153c, needle, red'
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.925
_reflns_odcompleteness_completeness 99.90
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C23A \\sim C23B: within 1A with sigma of 0.04 and sigma for terminal atoms of
0.08
3. Others
 Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H24A)=Sof(H24B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C22(H22C,H22D), C23A(H23A,H23B), C23B(H23C,H23D), C24(H24A,H24B),
 C24(H24C,H24D), C25(H25A,H25B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C13(H13), C15(H15), C16(H16)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              19869
_cell_oxdiff_length_a            8.3916(3)
_cell_oxdiff_length_b            11.1195(3)
_cell_oxdiff_length_c            12.5963(4)
_cell_oxdiff_angle_alpha         77.991(2)
_cell_oxdiff_angle_beta          75.246(3)
_cell_oxdiff_angle_gamma         75.627(3)
_cell_oxdiff_volume              1087.78(6)
_cell_oxdiff_measurement_reflns_used 13957