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_4086829
_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 H14 Cl3 Cr N4 S, 2(C3 H7 N O)'
_chemical_formula_sum            'C22 H28 Cl3 Cr N6 O2 S'
_chemical_formula_weight         598.91
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 90.030(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.724(7)
_cell_length_b                   10.973(2)
_cell_length_c                   14.001(3)
_cell_measurement_reflns_used    993
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.71
_cell_measurement_theta_min      3.56
_cell_volume                     5334.8(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8462
_diffrn_reflns_av_R_equivalents  0.1281
_diffrn_reflns_av_unetI/netI     0.1172
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30117
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        28.035
_diffrn_reflns_theta_max         28.035
_diffrn_reflns_theta_min         3.563
_diffrn_source                   'Daresbury SRS Station 16.2SMX'
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.10, Sheldrick, G.M., (2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.729
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.0070(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         7629
_refine_ls_number_restraints     2447
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0808
_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^)+(0.1381P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5355
_reflns_number_total             7629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00671_si_002.cif
_cod_data_source_block           '[Cr(15)Cl3]'
_cod_depositor_comments
'Adding full bibliography for 4086828--4086833.cif.'
_cod_database_code               4086829
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.960