Robust Chromium Precursors for Catalysis: Isolation and Structure of a Single-Component Ethylene Tetramerization Precatalyst.
Hirscher, Nathanael A.; Perez Sierra, Danny; Agapie, Theodor; Journal of the American Chemical Society 141 (2019) 6022–6029; doi:10.1021/jacs.9b01387

data_4128433
_publ_section_title
;
 Robust Chromium Precursors for Catalysis: Isolation and Structure of a
 Single-Component Ethylene Tetramerization Precatalyst.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6022
_journal_page_last               6029
_journal_paper_doi               10.1021/jacs.9b01387
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C27 H33 Cr O3'
_chemical_formula_sum            'C27 H33 Cr O3'
_chemical_formula_weight         457.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.754(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3974(4)
_cell_length_b                   22.6187(10)
_cell_length_c                   12.1007(5)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.36
_cell_measurement_theta_min      2.47
_cell_volume                     2295.73(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.09
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            87691
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.358
_diffrn_reflns_theta_min         2.889
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0631 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.9486. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.133
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         11083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+1.2046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8964
_reflns_number_total             11083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01387_si_001.cif
_cod_data_source_block           p17419_a
_cod_database_code               4128433
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.903
_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:
 C25(H25A,H25B), C18(H18A,H18B), C17(H17A,H17B), C10(H10A,H10B), C26(H26A,
 H26B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C15(H15), C12(H12), C13(H13), C22(H22), C14(H14), C21(H21), C6(H6),
 C5(H5), C4(H4), C7(H7), C20(H20)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              79333
_shelx_hkl_checksum              15699
_olex2_submission_special_instructions 'No special instructions were received'