Reversible, Room-Temperature C-C Bond Activation of Benzene by an Isolable Metal Complex.
Hicks, Jamie; Vasko, Petra; Goicoechea, Jose M.; Aldridge, Simon; Journal of the American Chemical Society 141 (2019) 11000–11003; doi:10.1021/jacs.9b05925

data_4127408
_publ_section_title
;
 Reversible, Room-Temperature C-C Bond Activation of Benzene by an
 Isolable Metal Complex.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11000
_journal_page_last               11003
_journal_paper_doi               10.1021/jacs.9b05925
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'C57 H70 Al N2 O, C18 H36 K N2 O6, 3.5(C6 H6)'
_chemical_formula_sum            'C96 H127 Al K N4 O7'
_chemical_formula_weight         1515.09
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90.502(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7012(5)
_cell_length_b                   15.1963(7)
_cell_length_c                   46.196(2)
_cell_measurement_reflns_used    7697
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      71.5630
_cell_measurement_theta_min      4.0540
_cell_volume                     8916.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            53858
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.425
_diffrn_reflns_theta_min         3.481
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_description       plate
_exptl_crystal_F_000             3276
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1431
_refine_ls_number_reflns         18411
_refine_ls_number_restraints     685
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0852
_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^)+(0.0718P)^2^+7.6403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11968
_reflns_number_total             18411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05925_si_004.cif
_cod_data_source_block           compound_4
_cod_database_code               4127408
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.811
_shelx_estimated_absorpt_t_max   0.960
_shelx_res_checksum              26748
_shelx_hkl_checksum              54058