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_4084006
_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         'C35 H37 Cr N2'
_chemical_formula_sum            'C42 H45 Cr N2'
_chemical_formula_weight         629.80
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                em_mr26
_audit_creation_date
;
'Thu Mar 27 11:28:41 2014'
;
_audit_update_record             'Thu Mar 27 11:46:56 CET 2014'
_cell_angle_alpha                90
_cell_angle_beta                 105.182(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3318(8)
_cell_length_b                   14.6278(6)
_cell_length_c                   28.7540(15)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      19.8890
_cell_measurement_theta_min      3.2830
_cell_volume                     7035.5(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -40.00   18.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6942   57.0000 -150.0000 116

  2 omega    1.00   88.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   57.0000 -120.0000 174

  3 omega  -10.00   89.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   77.0000  120.0000 198

  4 omega   -3.00   88.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   57.0000  -30.0000 182

  5 omega  -46.00   51.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -80.0000 -103.0190 194

  6 omega   -2.00   72.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   57.0000   60.0000 148

  7 omega  -51.00   49.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -77.0000  120.0000 200

  8 omega  -46.00   51.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -80.0000    5.8585 194

  9 omega  -51.00   49.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -77.0000  -60.0000 200

 10 omega   -3.00   88.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   57.0000   60.0000 182

 11 omega   -3.00   88.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723   57.0000    0.0000 182

 12 omega  -51.00   49.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       18.7723  -77.0000   90.0000 200

;
_diffrn_measurement_device       'four-circle 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      -0.0108282000
_diffrn_orient_matrix_UB_12      0.0006919000
_diffrn_orient_matrix_UB_13      -0.0255675000
_diffrn_orient_matrix_UB_21      0.0401844000
_diffrn_orient_matrix_UB_22      -0.0095065000
_diffrn_orient_matrix_UB_23      0.0001007000
_diffrn_orient_matrix_UB_31      -0.0081545000
_diffrn_orient_matrix_UB_32      -0.0475178000
_diffrn_orient_matrix_UB_33      -0.0003758000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2075
_diffrn_reflns_av_unetI/netI     0.1080
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            64076
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.146
_diffrn_reflns_theta_min         3.201
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       plate
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.2886
_exptl_crystal_size_mid          0.1153
_exptl_crystal_size_min          0.0222
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1074P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3913
_reflns_number_total             6292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500459k_si_002.cif
_cod_data_source_block           en_mr26_sq
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4084006
_audit_block_refno               2003
_audit_block_usercomment         'mr283, plate, green'
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.904
_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C20(H20),
 C21(H21), C24(H24), C25(H25), C27(H27), C28(H28), C31(H31), C32(H32), C34(H34),
  C35(H35)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              62313
_cell_oxdiff_length_a            17.3299(10)
_cell_oxdiff_length_b            14.6355(5)
_cell_oxdiff_length_c            28.7420(17)
_cell_oxdiff_angle_alpha         89.977(4)
_cell_oxdiff_angle_beta          105.180(5)
_cell_oxdiff_angle_gamma         89.951(4)
_cell_oxdiff_volume              7035.5(6)
_cell_oxdiff_measurement_reflns_used 3907
_reflns_odcompleteness_completeness 87.53
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1