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_4128430
_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         'C45 H45 Cr O3'
_chemical_formula_sum            'C45 H45 Cr O3'
_chemical_formula_weight         685.81
_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'
_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                 103.123(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5802(10)
_cell_length_b                   15.8845(12)
_cell_length_c                   20.0281(17)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.139
_cell_measurement_theta_min      2.618
_cell_volume                     3587.9(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      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0701
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            210362
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.313
_diffrn_reflns_theta_min         2.451
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.7082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0828 before and 0.0617 after correction. The Ratio of minimum to maximum transmission is 0.9479. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         17385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0586P)^2^+1.0790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13691
_reflns_number_total             17385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01387_si_001.cif
_cod_data_source_block           v18158_a
_cod_database_code               4128430
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.896
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C39(H39A,H39B), C24(H24A,H24B), C11(H11A,H11B), C38(H38A,
 H38B), C25(H25A,H25B), C37(H37A,H37B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C21(H21), C35(H35), C32(H32), C19(H19), C33(H33), C20(H20),
 C15(H15), C34(H34), C41(H41), C17(H17), C16(H16), C13(H13), C27(H27), C4(H4),
 C45(H45), C29(H29), C30(H30), C14(H14), C31(H31), C42(H42), C44(H44), C5(H5),
 C28(H28), C43(H43), C6(H6), C7(H7)
;
_shelx_res_checksum              7727
_shelx_hkl_checksum              35775
_olex2_submission_special_instructions 'No special instructions were received'