The long-sought seventeen-electron radical [(C6Me6)Cr(CO)3]+: isolation, crystal structure and substitution reaction
Wenqing Wang; Xingyong Wang; Zaichao Zhang; Ningning Yuan; Xinping Wang; Chem.Commun. 51 (2015) 8410–; doi:10.1039/C5cc01941A

data_7117147
_publ_section_title
;
 The long-sought seventeen-electron radical [(C6Me6)Cr(CO)3]+: isolation,
 crystal structure and substitution reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              8410
_journal_paper_doi               10.1039/C5cc01941A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C15 H18 Cr O3, C16 H12 Al F24 O4'
_chemical_formula_sum            'C31 H30 Al Cr F24 O7'
_chemical_formula_weight         1049.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-03 deposited with the CCDC.
2015-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.9130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.012(3)
_cell_length_b                   13.9336(15)
_cell_length_c                   25.099(3)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.28
_cell_volume                     8115.2(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX DUO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            65844
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.9262
_exptl_absorpt_correction_T_min  0.9139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2011)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.113
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2031
_refine_ls_number_reflns         17387
_refine_ls_number_restraints     3629
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+28.8115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2292
_refine_ls_wR_factor_ref         0.2434
_reflns_number_gt                13027
_reflns_number_total             17387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01941a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        8115.3(15)
_cod_original_sg_symbol_Hall     '-P 2yn  '
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               7117147