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_7117149
_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         'C32 H33 Cr O2 P'
_chemical_formula_sum            'C32 H33 Cr O2 P'
_chemical_formula_weight         532.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                90.671(7)
_cell_angle_beta                 99.551(7)
_cell_angle_gamma                116.355(7)
_cell_formula_units_Z            2
_cell_length_a                   8.649(4)
_cell_length_b                   9.593(4)
_cell_length_c                   17.771(8)
_cell_measurement_reflns_used    3269
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.34
_cell_volume                     1296.8(10)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.1143
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11036
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.838
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0832
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+3.7366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1916
_refine_ls_wR_factor_ref         0.2212
_reflns_number_gt                4166
_reflns_number_total             5799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc01941a2.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_Hall     '-P 1  '
_cod_original_sg_symbol_H-M      'P -1  '
_cod_database_code               7117149