Observation of Cationic Transition Metal-Alkane Complexes with Moderate Stability in Hydrofluorocarbon Solution.
Yau, Hon Man; McKay, Alasdair I.; Hesse, Henrique; Xu, Ran; He, Mushi; Holt, Camille E.; Ball, Graham E.; Journal of the American Chemical Society 138 (2016) 281–288; doi:10.1021/jacs.5b10583

data_4129807
_publ_section_title
;
 Observation of Cationic Transition Metal-Alkane Complexes with Moderate
 Stability in Hydrofluorocarbon Solution.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              281
_journal_page_last               288
_journal_paper_doi               10.1021/jacs.5b10583
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C37 H30 Al F36 O7 Re'
_chemical_formula_sum            'C37 H30 Al F36 O7 Re'
_chemical_formula_weight         1483.79
_chemical_name_common            '[Re(C6Et6)(CO)3][Al(OtBuF)4]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                91.371(3)
_cell_angle_beta                 90.174(3)
_cell_angle_gamma                95.164(4)
_cell_formula_units_Z            2
_cell_length_a                   10.7307(9)
_cell_length_b                   14.8887(13)
_cell_length_c                   15.7012(11)
_cell_measurement_temperature    150(2)
_cell_volume                     2497.6(3)
_computing_cell_refinement       'Bruker Apex II software'
_computing_data_collection       'Bruker Apex II software'
_computing_data_reduction        X-Seed
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2010'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37630
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.135
_diffrn_reflns_theta_min         1.297
_diffrn_source                   'Bruker Quazar Multilayer Optics'
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       'elongated tabular plate'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         6.466
_refine_diff_density_min         -1.893
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1307
_refine_ls_number_reflns         10885
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0671
_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^)+(0.1170P)^2^+5.3161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8932
_reflns_number_total             10885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10583_si_001.cif
_cod_data_source_block           added_by_encifer
_cod_database_code               4129807
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              32640
_shelx_hkl_checksum              56459