Metal-Mediated Controllable Creation of Secondary, Tertiary, and Quaternary Carbon Centers: A Powerful Strategy for the Synthesis of Iron, Cobalt, and Copper Complexes with in Situ Generated Substituted 1-Pyridineimidazo[1,5-a]pyridine Ligands
Yanmei Chen; Lei Li; Zhou Chen; Yonglu Liu; Hailiang Hu; Wenqian Chen; Wei Liu; Yahong Li; Tao Lei; Yanyuan Cao; Zhenghui Kang; Miaoshui Lin; Wu Li; Inorganic Chemistry 51 (2012) 9705–9713; doi:10.1021/ic300949y

data_4330328
_publ_section_title
;
 Metal-Mediated Controllable Creation of Secondary, Tertiary, and
 Quaternary Carbon Centers: A Powerful Strategy for the Synthesis of Iron,
 Cobalt, and Copper Complexes with in Situ Generated Substituted
 1-Pyridineimidazo[1,5-a]pyridine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9705
_journal_page_last               9713
_journal_paper_doi               10.1021/ic300949y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '2(C18 H12 Cl2 Co N4 O), C2 H6 O'
_chemical_formula_sum            'C38 H30 Cl4 Co2 N8 O3'
_chemical_formula_weight         906.36
_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                 100.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.499(3)
_cell_length_b                   14.100(3)
_cell_length_c                   16.128(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3689.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15976
_diffrn_reflns_theta_full        24.51
_diffrn_reflns_theta_max         24.51
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.7634
_exptl_absorpt_correction_T_min  0.7227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3064
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0992
_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^)+(0.1648P)^2^+31.2983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2685
_refine_ls_wR_factor_ref         0.2854
_reflns_number_gt                2565
_reflns_number_total             3064
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300949y_L1Co.cif
_cod_data_source_block           t
_cod_original_cell_volume        3689.2(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4330328