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_4128429
_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         'C42 H39 Cr O3'
_chemical_formula_sum            'C42 H39 Cr O3'
_chemical_formula_weight         643.73
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                95.481(2)
_cell_angle_beta                 102.260(2)
_cell_angle_gamma                115.318(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7286(4)
_cell_length_b                   11.7519(4)
_cell_length_c                   15.0753(5)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.36
_cell_measurement_theta_min      3.07
_cell_volume                     1641.19(11)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44667
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.435
_diffrn_reflns_theta_min         3.069
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.170
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0879 before and 0.0739 after correction. The Ratio of minimum to maximum transmission is 0.8447. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0265P)^2^+2.4140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4956
_reflns_number_total             6047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01387_si_001.cif
_cod_data_source_block           p17354
_cod_original_cell_volume        1641.19(10)
_cod_database_code               4128429
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.621
_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:
 C9(H9A,H9B), C10(H10A,H10B), C22(H22A,H22B), C23(H23A,H23B), C35(H35A,H35B),
 C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C38(H38),
 C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              6063
_shelx_hkl_checksum              84451
_olex2_submission_special_instructions 'No special instructions were received'