Group 3 Metal Complexes of Radical-Anionic 2,2'-Bipyridyl Ligands
Bryan N. Williams; Wenliang Huang; Kevin L. Miller; Paula L. Diaconescu; Inorganic Chemistry 49 (2010) 11493–11498; doi:10.1021/ic101493k

data_4317309
_publ_section_title
;
 Group 3 Metal Complexes of Radical-Anionic 2,2'-Bipyridyl Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11493
_journal_page_last               11498
_journal_paper_doi               10.1021/ic101493k
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '2(C44 H54 Fe Lu N4 Si2), C5 H6'
_chemical_formula_sum            'C93 H114 Fe2 Lu2 N8 Si4'
_chemical_formula_weight         1917.92
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.9540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.541(2)
_cell_length_b                   11.3868(14)
_cell_length_c                   22.597(3)
_cell_measurement_reflns_used    4867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.38
_cell_measurement_theta_min      3.93
_cell_volume                     4445.5(10)
_computing_cell_refinement       'Bruker APEX11'
_computing_data_collection       'Bruker APEX11'
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            38689
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    2.624
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.8176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.475
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         10934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+0.0124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                7763
_reflns_number_total             10934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101493k_si_003_2.cif
_cod_data_source_block           4Lu-pyPh
_cod_original_cell_volume        4445.6(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4317309