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_4127405
_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
;
C47 H62 Al Cl2 N2 O, C18 H36 K N2 O6, 2(C6 H6)
;
_chemical_formula_sum            'C77 H110 Al Cl2 K N4 O7'
_chemical_formula_weight         1340.66
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_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   geom
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_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_b                   12.8510(6)
_cell_length_c                   39.910(2)
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_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
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_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5035
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.1486
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            31395
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.218
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       needle
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         13750
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1585
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0684P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.2270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6796
_reflns_number_total             13750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05925_si_007.cif
_cod_data_source_block           compound_6
_cod_original_cell_volume        7513.2(8)
_cod_database_code               4127405
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.571
_shelx_estimated_absorpt_t_max   0.931
_shelx_res_checksum              81235
_shelx_hkl_checksum              95876