Alternating α-Olefin Distributions via Single and Double Insertions in Chromium-Catalyzed Ethylene Oligomerization
Tomov, Atanas K.; Nobbs, James D.; Chirinos, Juan J.; Saini, Prabhjot K.; Malinowski, Robert; Ho, Sarah K. Y.; Young, Craig T.; McGuinness, David S.; White, Andrew J. P.; Elsegood, Mark R. J.; Britovsek, George J. P.; Organometallics 36 (2016) 510–; doi:10.1021/acs.organomet.6b00671

data_4086831
_publ_section_title
;
 Alternating \a-Olefin Distributions via Single and Double Insertions in
 Chromium-Catalyzed Ethylene Oligomerization
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              510
_journal_paper_doi               10.1021/acs.organomet.6b00671
_journal_volume                  36
_journal_year                    2016
_chemical_formula_moiety         'C16 H17 Cl2 Cr N5 O, F6 Sb, 3.5(C4 H8 O)'
_chemical_formula_sum            'C30 H45 Cl2 Cr F6 N5 O4.5 Sb'
_chemical_formula_weight         906.36
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL
_cell_angle_alpha                83.657(3)
_cell_angle_beta                 65.315(3)
_cell_angle_gamma                82.386(3)
_cell_formula_units_Z            2
_cell_length_a                   13.2253(4)
_cell_length_b                   13.2985(4)
_cell_length_c                   14.7851(5)
_cell_measurement_reflns_used    9556
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.7580
_cell_measurement_theta_min      4.3160
_cell_volume                     2337.50(14)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9863
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28390
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.204
_diffrn_reflns_theta_min         4.085
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.982
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Pale aquamarine'
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       prisms
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
 SQUEEZE suggested 269 e/cell = 134.5 e/asu
 The solvents used were thf (C4H8O, 40e) and heptane (C7H16, 58e)
 Before the use of SQUEEZE the solvent was clearly thf
 3.5(C4H8O) = 140e, so this was used as the solvent present
 
 So, the atom list is low by 3.5(C4H8O) = C14 H28 O3.5, and the UNIT is
 low by C28 H56 O7. Combined with the missing aqua protons
 the UNIT is low by C28 H60 O7, i.e. C32 H30 N10 O2 F12 Cl4 Cr2 Sb2
 
 The missing 18 non-H atoms in the asu would have required 162 variables
 (18 x 9) if refined anisotropically.
 The L.S. instruction was adjusted appropriately.
;
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.0100(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         17187
_refine_ls_number_restraints     1518
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1156P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9748
_reflns_number_total             17187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00671_si_002.cif
_cod_data_source_block           Cr-1-Cl2-OH2_SbF6
_cod_depositor_comments
'Adding full bibliography for 4086828--4086833.cif.'
_cod_original_cell_volume        2337.51(15)
_cod_original_formula_sum        'C30 H45 Cl2 Cr F6 N5 O4.50 Sb'
_cod_database_code               4086831
_shelxl_version_number           2013-4