#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:17:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179406 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/03/4330332.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4330332
loop_
_publ_author_name
'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'
_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         'C36 H26 Cl4 Fe2 N8'
_chemical_formula_sum            'C36 H26 Cl4 Fe2 N8'
_chemical_formula_weight         824.15
_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
_cell_angle_alpha                89.205(2)
_cell_angle_beta                 84.970(2)
_cell_angle_gamma                82.380(2)
_cell_formula_units_Z            1
_cell_length_a                   9.2174(4)
_cell_length_b                   9.4861(4)
_cell_length_c                   9.9179(4)
_cell_measurement_reflns_used    4869
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.24
_cell_volume                     856.22(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14044
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  0.8129
_exptl_absorpt_correction_T_min  0.7534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0444P)²+0.1895P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                2596
_reflns_number_total             3377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300949y_L2Fe.cif
_cod_data_source_block           3
_cod_database_code               4330332
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.26420(3) 0.72669(3) 0.24186(3) 0.04364(13) Uani 1 1 d .
Cl1 Cl 0.44568(8) 0.86711(7) 0.18971(8) 0.0665(2) Uani 1 1 d .
Cl2 Cl 0.18301(8) 0.75433(8) 0.46935(7) 0.0677(2) Uani 1 1 d .
N2 N 0.22144(18) 0.64426(19) 0.05685(18) 0.0392(4) Uani 1 1 d .
N4 N 0.38801(19) 0.49831(19) 0.25996(18) 0.0405(4) Uani 1 1 d .
N3 N 0.08521(18) 0.61725(19) -0.11036(18) 0.0393(4) Uani 1 1 d .
C12 C 0.2922(2) 0.5349(2) -0.0204(2) 0.0373(5) Uani 1 1 d .
C14 C 0.4265(2) 0.4027(2) 0.1594(2) 0.0379(5) Uani 1 1 d .
C10 C 0.2247(3) 0.4165(3) -0.2346(2) 0.0445(6) Uani 1 1 d .
H10 H 0.3067 0.3478 -0.2460 0.053 Uiso 1 1 calc R
N1 N 0.0518(2) 0.8475(2) 0.1857(2) 0.0471(5) Uani 1 1 d .
C13 C 0.4353(2) 0.4553(2) 0.0142(2) 0.0376(5) Uani 1 1 d .
H13 H 0.4562 0.3714 -0.0444 0.045 Uiso 1 1 calc R
C11 C 0.2104(2) 0.5141(2) -0.1268(2) 0.0388(5) Uani 1 1 d .
C6 C 0.0965(2) 0.6933(2) 0.0031(2) 0.0387(5) Uani 1 1 d .
C7 C -0.0212(3) 0.6236(3) -0.2027(2) 0.0508(6) Uani 1 1 d .
H7 H -0.1032 0.6925 -0.1941 0.061 Uiso 1 1 calc R
C18 C 0.3901(3) 0.4490(3) 0.3876(2) 0.0485(6) Uani 1 1 d .
H18 H 0.3651 0.5139 0.4580 0.058 Uiso 1 1 calc R
C1 C -0.0014(2) 0.8093(2) 0.0714(2) 0.0415(5) Uani 1 1 d .
C8 C -0.0039(3) 0.5294(3) -0.3039(3) 0.0568(7) Uani 1 1 d .
H8 H -0.0753 0.5340 -0.3651 0.068 Uiso 1 1 calc R
C15 C 0.4595(3) 0.2594(3) 0.1858(3) 0.0492(6) Uani 1 1 d .
H15 H 0.4816 0.1953 0.1145 0.059 Uiso 1 1 calc R
C2 C -0.1332(3) 0.8754(3) 0.0297(3) 0.0515(6) Uani 1 1 d .
H2 H -0.1683 0.8475 -0.0495 0.062 Uiso 1 1 calc R
C17 C 0.4272(3) 0.3078(3) 0.4204(3) 0.0557(7) Uani 1 1 d .
H17 H 0.4301 0.2790 0.5103 0.067 Uiso 1 1 calc R
C16 C 0.4597(3) 0.2110(3) 0.3172(3) 0.0575(7) Uani 1 1 d .
H16 H 0.4816 0.1145 0.3356 0.069 Uiso 1 1 calc R
C9 C 0.1189(3) 0.4235(3) -0.3209(2) 0.0535(6) Uani 1 1 d .
H9 H 0.1269 0.3586 -0.3915 0.064 Uiso 1 1 calc R
C4 C -0.1583(3) 1.0233(3) 0.2244(3) 0.0636(7) Uani 1 1 d .
H4 H -0.2099 1.0959 0.2783 0.076 Uiso 1 1 calc R
C5 C -0.0264(3) 0.9528(3) 0.2594(3) 0.0580(7) Uani 1 1 d .
H5 H 0.0101 0.9799 0.3382 0.070 Uiso 1 1 calc R
C3 C -0.2111(3) 0.9837(3) 0.1082(3) 0.0590(7) Uani 1 1 d .
H3 H -0.2998 1.0296 0.0820 0.071 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Fe1 N1 73.27(7) . .
N2 Fe1 Cl1 105.39(5) . .
N1 Fe1 Cl1 107.70(6) . .
N2 Fe1 Cl2 144.89(6) . .
N1 Fe1 Cl2 89.88(5) . .
Cl1 Fe1 Cl2 109.07(3) . .
N2 Fe1 N4 80.85(7) . .
N1 Fe1 N4 142.70(7) . .
Cl1 Fe1 N4 104.74(5) . .
Cl2 Fe1 N4 96.56(5) . .
C6 N2 C12 108.53(17) . .
C6 N2 Fe1 119.12(14) . .
C12 N2 Fe1 132.03(14) . .
C18 N4 C14 117.1(2) . .
C18 N4 Fe1 114.08(15) . .
C14 N4 Fe1 126.98(15) . .
C6 N3 C7 132.93(19) . .
C6 N3 C11 107.44(17) . .
C7 N3 C11 119.63(19) . .
N2 C12 C11 109.19(18) . .
N2 C12 C13 121.73(18) . .
C11 C12 C13 129.08(19) . .
N4 C14 C15 121.7(2) . .
N4 C14 C13 118.80(19) . .
C15 C14 C13 119.5(2) . .
C9 C10 C11 119.6(2) . .
C9 C10 H10 120.2 . .
C11 C10 H10 120.2 . .
C5 N1 C1 118.1(2) . .
C5 N1 Fe1 124.33(17) . .
C1 N1 Fe1 117.61(14) . .
C12 C13 C14 111.54(17) . .
C12 C13 C13 112.0(2) . 2_665
C14 C13 C13 110.9(2) . 2_665
C12 C13 H13 107.4 . .
C14 C13 H13 107.4 . .
C13 C13 H13 107.4 2_665 .
C12 C11 C10 135.0(2) . .
C12 C11 N3 105.46(18) . .
C10 C11 N3 119.53(19) . .
N2 C6 N3 109.38(18) . .
N2 C6 C1 118.67(19) . .
N3 C6 C1 131.94(19) . .
C8 C7 N3 119.2(2) . .
C8 C7 H7 120.4 . .
N3 C7 H7 120.4 . .
N4 C18 C17 123.9(2) . .
N4 C18 H18 118.1 . .
C17 C18 H18 118.1 . .
N1 C1 C2 121.9(2) . .
N1 C1 C6 111.21(18) . .
C2 C1 C6 126.9(2) . .
C7 C8 C9 122.2(2) . .
C7 C8 H8 118.9 . .
C9 C8 H8 118.9 . .
C16 C15 C14 120.2(2) . .
C16 C15 H15 119.9 . .
C14 C15 H15 119.9 . .
C3 C2 C1 118.5(2) . .
C3 C2 H2 120.8 . .
C1 C2 H2 120.8 . .
C16 C17 C18 118.3(2) . .
C16 C17 H17 120.8 . .
C18 C17 H17 120.8 . .
C17 C16 C15 118.7(2) . .
C17 C16 H16 120.6 . .
C15 C16 H16 120.6 . .
C10 C9 C8 119.8(2) . .
C10 C9 H9 120.1 . .
C8 C9 H9 120.1 . .
C3 C4 C5 118.1(2) . .
C3 C4 H4 120.9 . .
C5 C4 H4 120.9 . .
N1 C5 C4 123.3(3) . .
N1 C5 H5 118.4 . .
C4 C5 H5 118.4 . .
C4 C3 C2 120.1(2) . .
C4 C3 H3 119.9 . .
C2 C3 H3 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 2.0934(17) .
Fe1 N1 2.2440(19) .
Fe1 Cl1 2.2934(7) .
Fe1 Cl2 2.3211(7) .
Fe1 N4 2.3233(18) .
N2 C6 1.336(3) .
N2 C12 1.358(3) .
N4 C18 1.345(3) .
N4 C14 1.349(3) .
N3 C6 1.364(3) .
N3 C7 1.395(3) .
N3 C11 1.410(3) .
C12 C11 1.380(3) .
C12 C13 1.496(3) .
C14 C15 1.380(3) .
C14 C13 1.516(3) .
C10 C9 1.348(3) .
C10 C11 1.410(3) .
C10 H10 0.9300 .
N1 C5 1.338(3) .
N1 C1 1.346(3) .
C13 C13 1.557(4) 2_665
C13 H13 0.9800 .
C6 C1 1.461(3) .
C7 C8 1.338(4) .
C7 H7 0.9300 .
C18 C17 1.379(3) .
C18 H18 0.9300 .
C1 C2 1.385(3) .
C8 C9 1.411(4) .
C8 H8 0.9300 .
C15 C16 1.376(4) .
C15 H15 0.9300 .
C2 C3 1.381(4) .
C2 H2 0.9300 .
C17 C16 1.372(3) .
C17 H17 0.9300 .
C16 H16 0.9300 .
C9 H9 0.9300 .
C4 C3 1.365(4) .
C4 C5 1.378(4) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C3 H3 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C13 H13 Cl1 0.98 2.71 3.679(2) 171.1 2_665
C18 H18 Cl2 0.93 2.64 3.320(3) 130.0 .
