#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:20:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179447 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/44/4334479.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_4334479
loop_
_publ_author_name
'Mei Wang'
'Jason England'
'Thomas Weyhermüller'
'Swarna-Latha Kokatam'
'Christopher J. Pollock'
'Serena DeBeer'
'Jingmei Shen'
'Glenn P.A. Yap'
'Klaus H. Theopold'
'Karl Wieghardt'
_publ_section_title
;
 New Complexes of Chromium(III) Containing Organic π-Radical Ligands: An
 Experimental and Density Functional Theory Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4472
_journal_page_last               4487
_journal_paper_doi               10.1021/ic302743s
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C42 H72 Cr N6'
_chemical_formula_sum            'C42 H72 Cr N6'
_chemical_formula_weight         713.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   17.205(2)
_cell_length_b                   17.205(2)
_cell_length_c                   46.944(8)
_cell_measurement_temperature    200(2)
_cell_volume                     12034(3)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       ω
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            43776
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.9692
_exptl_absorpt_correction_T_min  0.9488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       block
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0446
_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/[σ²(Fo²)+(0.0443P)²+25.5977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1124
_reflns_number_gt                2748
_reflns_number_total             3340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302743s_si_002_4.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4334479
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
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
Cr Cr 0.0000 0.0000 0.121577(9) 0.01883(12) Uani 1 3 d S
N1 N -0.02465(9) 0.08395(9) 0.14555(3) 0.0222(3) Uani 1 1 d .
N2 N 0.06183(9) 0.11501(9) 0.09805(3) 0.0219(3) Uani 1 1 d .
C1 C 0.01090(11) 0.16676(11) 0.13509(4) 0.0277(3) Uani 1 1 d .
H1A H 0.0050 0.2122 0.1446 0.033 Uiso 1 1 calc R
C2 C 0.05706(11) 0.18325(11) 0.10950(4) 0.0280(4) Uani 1 1 d .
H2A H 0.0839 0.2405 0.1006 0.034 Uiso 1 1 calc R
C3 C -0.04113(12) 0.13855(13) 0.19411(4) 0.0346(4) Uani 1 1 d .
H3A H 0.0225 0.1583 0.1983 0.042 Uiso 1 1 calc R
H3B H -0.0442 0.1905 0.1863 0.042 Uiso 1 1 calc R
C4 C -0.09618(15) 0.10617(16) 0.22151(4) 0.0437(5) Uani 1 1 d .
H4A H -0.0913 0.0557 0.2296 0.052 Uiso 1 1 calc R
H4B H -0.0721 0.1554 0.2357 0.052 Uiso 1 1 calc R
C5 C -0.19435(14) 0.07574(14) 0.21560(4) 0.0384(4) Uani 1 1 d .
H5A H -0.2294 0.0526 0.2334 0.046 Uiso 1 1 calc R
H5B H -0.1997 0.1276 0.2091 0.046 Uiso 1 1 calc R
C6 C -0.23248(13) 0.00277(13) 0.19298(4) 0.0383(4) Uani 1 1 d .
H6A H -0.2945 -0.0120 0.1884 0.046 Uiso 1 1 calc R
H6B H -0.2349 -0.0521 0.2006 0.046 Uiso 1 1 calc R
C7 C -0.17602(11) 0.03160(12) 0.16575(4) 0.0299(4) Uani 1 1 d .
H7A H -0.1805 0.0810 0.1566 0.036 Uiso 1 1 calc R
H7B H -0.1999 -0.0195 0.1523 0.036 Uiso 1 1 calc R
C8 C -0.07733(11) 0.06290(11) 0.17208(3) 0.0241(3) Uani 1 1 d .
H8A H -0.0757 0.0111 0.1811 0.029 Uiso 1 1 calc R
C9 C 0.10943(13) 0.19395(13) 0.05017(4) 0.0343(4) Uani 1 1 d .
H9A H 0.1307 0.2540 0.0586 0.041 Uiso 1 1 calc R
H9B H 0.0458 0.1688 0.0446 0.041 Uiso 1 1 calc R
C10 C 0.16551(13) 0.20269(14) 0.02372(4) 0.0391(4) Uani 1 1 d .
H10A H 0.1411 0.1432 0.0145 0.047 Uiso 1 1 calc R
H10B H 0.1612 0.2439 0.0099 0.047 Uiso 1 1 calc R
C11 C 0.26332(13) 0.23819(14) 0.03130(4) 0.0405(5) Uani 1 1 d .
H11A H 0.2898 0.3004 0.0385 0.049 Uiso 1 1 calc R
H11B H 0.2968 0.2393 0.0140 0.049 Uiso 1 1 calc R
C12 C 0.27243(13) 0.17975(15) 0.05390(4) 0.0395(5) Uani 1 1 d .
H12A H 0.3362 0.2070 0.0596 0.047 Uiso 1 1 calc R
H12B H 0.2534 0.1198 0.0458 0.047 Uiso 1 1 calc R
C13 C 0.21552(11) 0.16937(14) 0.08020(4) 0.0335(4) Uani 1 1 d .
H13A H 0.2202 0.1281 0.0939 0.040 Uiso 1 1 calc R
H13C H 0.2389 0.2284 0.0896 0.040 Uiso 1 1 calc R
C14 C 0.11725(11) 0.13261(11) 0.07226(3) 0.0244(3) Uani 1 1 d .
H14A H 0.0964 0.0734 0.0628 0.029 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'
Cr Cr 0.3209 0.6236 '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
N1 Cr N1 92.40(5) 2 3
N1 Cr N1 92.40(5) 2 .
N1 Cr N1 92.40(5) 3 .
N1 Cr N2 78.67(5) 2 2
N1 Cr N2 167.42(5) 3 2
N1 Cr N2 96.77(5) . 2
N1 Cr N2 96.77(5) 2 3
N1 Cr N2 78.67(5) 3 3
N1 Cr N2 167.42(5) . 3
N2 Cr N2 93.47(5) 2 3
N1 Cr N2 167.42(5) 2 .
N1 Cr N2 96.77(5) 3 .
N1 Cr N2 78.67(5) . .
N2 Cr N2 93.47(5) 2 .
N2 Cr N2 93.47(5) 3 .
C1 N1 C8 118.11(13) . .
C1 N1 Cr 114.08(11) . .
C8 N1 Cr 127.80(10) . .
C2 N2 C14 117.96(13) . .
C2 N2 Cr 113.89(10) . .
C14 N2 Cr 127.82(10) . .
N1 C1 C2 116.57(15) . .
N1 C1 H1A 121.7 . .
C2 C1 H1A 121.7 . .
N2 C2 C1 116.76(15) . .
N2 C2 H2A 121.6 . .
C1 C2 H2A 121.6 . .
C4 C3 C8 110.14(16) . .
C4 C3 H3A 109.6 . .
C8 C3 H3A 109.6 . .
C4 C3 H3B 109.6 . .
C8 C3 H3B 109.6 . .
H3A C3 H3B 108.1 . .
C5 C4 C3 110.54(16) . .
C5 C4 H4A 109.5 . .
C3 C4 H4A 109.5 . .
C5 C4 H4B 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 108.1 . .
C6 C5 C4 110.96(16) . .
C6 C5 H5A 109.4 . .
C4 C5 H5A 109.4 . .
C6 C5 H5B 109.4 . .
C4 C5 H5B 109.4 . .
H5A C5 H5B 108.0 . .
C5 C6 C7 111.96(15) . .
C5 C6 H6A 109.2 . .
C7 C6 H6A 109.2 . .
C5 C6 H6B 109.2 . .
C7 C6 H6B 109.2 . .
H6A C6 H6B 107.9 . .
C6 C7 C8 111.37(15) . .
C6 C7 H7A 109.4 . .
C8 C7 H7A 109.4 . .
C6 C7 H7B 109.4 . .
C8 C7 H7B 109.4 . .
H7A C7 H7B 108.0 . .
N1 C8 C3 115.03(14) . .
N1 C8 C7 111.08(13) . .
C3 C8 C7 109.76(13) . .
N1 C8 H8A 106.8 . .
C3 C8 H8A 106.8 . .
C7 C8 H8A 106.8 . .
C14 C9 C10 110.36(15) . .
C14 C9 H9A 109.6 . .
C10 C9 H9A 109.6 . .
C14 C9 H9B 109.6 . .
C10 C9 H9B 109.6 . .
H9A C9 H9B 108.1 . .
C11 C10 C9 111.49(15) . .
C11 C10 H10A 109.3 . .
C9 C10 H10A 109.3 . .
C11 C10 H10B 109.3 . .
C9 C10 H10B 109.3 . .
H10A C10 H10B 108.0 . .
C10 C11 C12 110.93(16) . .
C10 C11 H11A 109.5 . .
C12 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
C12 C11 H11B 109.5 . .
H11A C11 H11B 108.0 . .
C11 C12 C13 111.61(16) . .
C11 C12 H12A 109.3 . .
C13 C12 H12A 109.3 . .
C11 C12 H12B 109.3 . .
C13 C12 H12B 109.3 . .
H12A C12 H12B 108.0 . .
C14 C13 C12 111.28(14) . .
C14 C13 H13A 109.4 . .
C12 C13 H13A 109.4 . .
C14 C13 H13C 109.4 . .
C12 C13 H13C 109.4 . .
H13A C13 H13C 108.0 . .
N2 C14 C13 110.65(13) . .
N2 C14 C9 115.23(13) . .
C13 C14 C9 109.92(14) . .
N2 C14 H14A 106.9 . .
C13 C14 H14A 106.9 . .
C9 C14 H14A 106.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr N1 2.0359(13) 2
Cr N1 2.0359(13) 3
Cr N1 2.0359(13) .
Cr N2 2.0399(13) 2
Cr N2 2.0399(13) 3
Cr N2 2.0400(13) .
N1 C1 1.332(2) .
N1 C8 1.4749(19) .
N2 C2 1.330(2) .
N2 C14 1.4759(19) .
C1 C2 1.389(2) .
C1 H1A 0.9500 .
C2 H2A 0.9500 .
C3 C4 1.528(3) .
C3 C8 1.530(2) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.523(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.520(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.530(2) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.532(2) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 1.0000 .
C9 C14 1.533(2) .
C9 C10 1.533(2) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.518(3) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.523(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.530(2) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.526(2) .
C13 H13A 0.9900 .
C13 H13C 0.9900 .
C14 H14A 1.0000 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
N1 Cr N1 C1 -172.40(12) 2
N1 Cr N1 C1 95.10(14) 3
N2 Cr N1 C1 -93.53(12) 2
N2 Cr N1 C1 50.8(3) 3
N2 Cr N1 C1 -1.33(11) .
N1 Cr N1 C8 6.42(13) 2
N1 Cr N1 C8 -86.09(10) 3
N2 Cr N1 C8 85.28(13) 2
N2 Cr N1 C8 -130.4(2) 3
N2 Cr N1 C8 177.49(13) .
N1 Cr N2 C2 46.5(3) 2
N1 Cr N2 C2 -90.03(12) 3
N1 Cr N2 C2 1.07(11) .
N2 Cr N2 C2 97.29(14) 2
N2 Cr N2 C2 -169.02(12) 3
N1 Cr N2 C14 -140.3(2) 2
N1 Cr N2 C14 83.19(13) 3
N1 Cr N2 C14 174.29(13) .
N2 Cr N2 C14 -89.50(10) 2
N2 Cr N2 C14 4.20(13) 3
C8 N1 C1 C2 -177.53(14) .
Cr N1 C1 C2 1.40(19) .
C14 N2 C2 C1 -174.61(14) .
Cr N2 C2 C1 -0.67(19) .
N1 C1 C2 N2 -0.5(2) .
C8 C3 C4 C5 -59.5(2) .
C3 C4 C5 C6 56.8(2) .
C4 C5 C6 C7 -54.1(2) .
C5 C6 C7 C8 54.1(2) .
C1 N1 C8 C3 -37.5(2) .
Cr N1 C8 C3 143.73(12) .
C1 N1 C8 C7 87.95(17) .
Cr N1 C8 C7 -90.82(15) .
C4 C3 C8 N1 -175.07(14) .
C4 C3 C8 C7 58.81(19) .
C6 C7 C8 N1 175.63(14) .
C6 C7 C8 C3 -56.03(19) .
C14 C9 C10 C11 -57.4(2) .
C9 C10 C11 C12 55.5(2) .
C10 C11 C12 C13 -54.4(2) .
C11 C12 C13 C14 55.6(2) .
C2 N2 C14 C13 84.08(18) .
Cr N2 C14 C13 -88.89(16) .
C2 N2 C14 C9 -41.4(2) .
Cr N2 C14 C9 145.65(13) .
C12 C13 C14 N2 174.73(15) .
C12 C13 C14 C9 -56.9(2) .
C10 C9 C14 N2 -176.68(14) .
C10 C9 C14 C13 57.5(2) .
