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_4128431
_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         '0.5(C42 H42 Cr2 O6)'
_chemical_formula_sum            'C21 H21 Cr O3'
_chemical_formula_weight         373.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                75.513(5)
_cell_angle_beta                 87.541(5)
_cell_angle_gamma                80.203(5)
_cell_formula_units_Z            4
_cell_length_a                   12.0150(16)
_cell_length_b                   12.4851(16)
_cell_length_c                   15.1703(19)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.15
_cell_measurement_theta_min      2.38
_cell_volume                     2171.2(5)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.899
_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  0.0687
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            102156
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.171
_diffrn_reflns_theta_min         2.210
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0728 before and 0.0604 after correction. The Ratio of minimum to maximum transmission is 0.9549. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         14945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+2.8862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11010
_reflns_number_total             14945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01387_si_001.cif
_cod_data_source_block           v18078_a2_sq
_cod_database_code               4128431
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16),
 C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28),
  C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C30(H30A,H30B,
 H30C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              81779
_shelx_hkl_checksum              42791
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_olex2_submission_special_instructions 'No special instructions were received'