A Homologous Series of Cobalt, Rhodium, and Iridium Metalloradicals
Ayumi Takaoka; Jonas C. Peters; Inorganic Chemistry 51 (2012) 16–18; doi:10.1021/ic202079r

data_4327867
_publ_section_title
;
 A Homologous Series of Cobalt, Rhodium, and Iridium Metalloradicals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              16
_journal_page_last               18
_journal_paper_doi               10.1021/ic202079r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C71 H75 B F24 P4 Rh Si'
_chemical_formula_weight         1650.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.083(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.898(2)
_cell_length_b                   14.9266(10)
_cell_length_c                   29.4282(19)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.16
_cell_volume                     16047.5(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            211474
_diffrn_reflns_theta_full        30.58
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       blade
_exptl_crystal_F_000             6728
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.569
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         24573
_refine_ls_number_restraints     816
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1198P)^2^+82.4666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1931
_reflns_number_gt                17685
_reflns_number_total             24573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202079r_si_002_2.cif
_cod_data_source_block           ayt16try2
_cod_original_cell_volume        16047.7(18)
_cod_database_code               4327867