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_4330335
_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         'C42 H28 Cl4 Fe2 N10, C2 H6 O'
_chemical_formula_sum            'C44 H34 Cl4 Fe2 N10 O'
_chemical_formula_weight         972.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.551(5)
_cell_length_b                   14.520(4)
_cell_length_c                   18.101(5)
_cell_measurement_reflns_used    1923
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.437
_cell_measurement_theta_min      2.805
_cell_volume                     4613(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0539
_diffrn_reflns_av_sigmaI/netI    0.0583
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33054
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.8052
_exptl_absorpt_correction_T_min  0.7855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8200
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+7.0417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2143
_reflns_number_gt                6232
_reflns_number_total             8200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300949y_L3-Fe.cif
_cod_data_source_block           t
_cod_database_code               4330335