#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:20:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179447 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/44/4334476.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_4334476
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_compound_source        'benzene, hexane'
_chemical_formula_moiety         'C24 H22 Cr N4 O4'
_chemical_formula_sum            'C24 H22 Cr N4 O4'
_chemical_formula_weight         482.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_block_code                WGT-WM-002-08
_audit_creation_date             2012-09-14
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.117(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0904(11)
_cell_length_b                   18.019(3)
_cell_length_c                   15.221(2)
_cell_measurement_reflns_used    8470
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5451
_cell_measurement_theta_min      2.2605
_cell_volume                     2169.5(5)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29229
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.98427
_exptl_absorpt_correction_T_min  0.91545
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         3179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0440P)²+3.0953P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                2675
_reflns_number_total             3179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302743s_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4334476
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.5000 0.714443(19) 0.7500 0.01227(10) Uani 1 2 d S
N1 N 0.43704(16) 0.79909(7) 0.82610(8) 0.0138(2) Uani 1 1 d .
C2 C 0.2839(2) 0.83277(9) 0.81471(10) 0.0174(3) Uani 1 1 d .
H2 H 0.1896 0.8097 0.7769 0.021 Uiso 1 1 calc R
C3 C 0.2592(2) 0.89875(10) 0.85546(11) 0.0218(3) Uani 1 1 d .
H3 H 0.1504 0.9210 0.8450 0.026 Uiso 1 1 calc R
C4 C 0.3960(2) 0.93248(10) 0.91239(12) 0.0233(3) Uani 1 1 d .
H4 H 0.3824 0.9786 0.9403 0.028 Uiso 1 1 calc R
C5 C 0.5518(2) 0.89786(9) 0.92768(11) 0.0199(3) Uani 1 1 d .
H5 H 0.6455 0.9190 0.9681 0.024 Uiso 1 1 calc R
C6 C 0.57046(19) 0.83162(8) 0.88340(10) 0.0147(3) Uani 1 1 d .
C7 C 0.72881(19) 0.79123(8) 0.89288(10) 0.0147(3) Uani 1 1 d .
C8 C 0.8799(2) 0.81275(9) 0.95046(10) 0.0184(3) Uani 1 1 d .
H8 H 0.8831 0.8552 0.9877 0.022 Uiso 1 1 calc R
C9 C 1.0236(2) 0.77137(10) 0.95221(11) 0.0218(3) Uani 1 1 d .
H9 H 1.1276 0.7856 0.9901 0.026 Uiso 1 1 calc R
C10 C 1.0155(2) 0.70825(10) 0.89777(11) 0.0209(3) Uani 1 1 d .
H10 H 1.1140 0.6796 0.8973 0.025 Uiso 1 1 calc R
C11 C 0.8620(2) 0.68846(9) 0.84494(11) 0.0173(3) Uani 1 1 d .
H11 H 0.8556 0.6446 0.8098 0.021 Uiso 1 1 calc R
N12 N 0.71987(16) 0.72913(7) 0.84111(8) 0.0139(2) Uani 1 1 d .
O21 O 0.60736(14) 0.64014(6) 0.68528(7) 0.0168(2) Uani 1 1 d .
C22 C 0.5443(2) 0.58012(9) 0.64542(10) 0.0171(3) Uani 1 1 d .
O23 O 0.39270(16) 0.56520(7) 0.62260(9) 0.0249(3) Uani 1 1 d .
C24 C 0.6746(2) 0.52639(10) 0.62502(15) 0.0308(4) Uani 1 1 d .
H24A H 0.7123 0.4937 0.6768 0.046 Uiso 1 1 calc R
H24B H 0.7714 0.5541 0.6127 0.046 Uiso 1 1 calc R
H24C H 0.6244 0.4965 0.5723 0.046 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 0.00 0.0150
0.00 1.00 0.00 0.0150
-1.00 -1.00 1.00 0.0450
1.00 1.00 -1.00 0.0450
0.00 1.00 -2.00 0.0700
0.00 -1.00 2.00 0.0800
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
O21 Cr O21 94.31(7) 2_656 .
O21 Cr N12 90.86(5) 2_656 2_656
O21 Cr N12 99.33(5) . 2_656
O21 Cr N12 99.33(5) 2_656 .
O21 Cr N12 90.87(5) . .
N12 Cr N12 165.02(7) 2_656 .
O21 Cr N1 92.02(5) 2_656 .
O21 Cr N1 168.48(5) . .
N12 Cr N1 90.17(5) 2_656 .
N12 Cr N1 78.61(5) . .
O21 Cr N1 168.48(5) 2_656 2_656
O21 Cr N1 92.02(5) . 2_656
N12 Cr N1 78.61(5) 2_656 2_656
N12 Cr N1 90.17(5) . 2_656
N1 Cr N1 83.43(7) . 2_656
C2 N1 C6 117.80(13) . .
C2 N1 Cr 126.20(10) . .
C6 N1 Cr 115.07(10) . .
N1 C2 C3 122.96(15) . .
C2 C3 C4 119.08(16) . .
C5 C4 C3 119.01(15) . .
C4 C5 C6 119.52(15) . .
N1 C6 C5 121.56(14) . .
N1 C6 C7 114.17(13) . .
C5 C6 C7 124.27(14) . .
N12 C7 C8 121.52(14) . .
N12 C7 C6 114.53(13) . .
C8 C7 C6 123.94(14) . .
C9 C8 C7 118.98(15) . .
C8 C9 C10 119.59(15) . .
C11 C10 C9 118.70(15) . .
N12 C11 C10 122.58(15) . .
C11 N12 C7 118.56(13) . .
C11 N12 Cr 124.97(11) . .
C7 N12 Cr 115.77(10) . .
C22 O21 Cr 129.22(10) . .
O23 C22 O21 125.92(15) . .
O23 C22 C24 119.88(15) . .
O21 C22 C24 114.18(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr O21 1.9690(11) 2_656
Cr O21 1.9690(11) .
Cr N12 2.0302(13) 2_656
Cr N12 2.0302(13) .
Cr N1 2.0434(13) .
Cr N1 2.0434(13) 2_656
N1 C2 1.357(2) .
N1 C6 1.3690(19) .
C2 C3 1.375(2) .
C3 C4 1.394(2) .
C4 C5 1.381(2) .
C5 C6 1.394(2) .
C6 C7 1.454(2) .
C7 N12 1.3619(19) .
C7 C8 1.401(2) .
C8 C9 1.377(2) .
C9 C10 1.401(2) .
C10 C11 1.377(2) .
C11 N12 1.355(2) .
O21 C22 1.2914(19) .
C22 O23 1.232(2) .
C22 C24 1.510(2) .
