# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Cr-7-Cl3
_database_code_depnum_ccdc_archive 'CCDC 1473101'
_audit_update_record             
;
2016-04-08 deposited with the CCDC.
2018-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H19 Cl3 Cr N5, 2(C3 H7 N O)'
_chemical_formula_sum            'C27 H33 Cl3 Cr N7 O2'
_chemical_formula_weight         645.95

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   18.2412(2)
_cell_length_b                   14.5616(2)
_cell_length_c                   23.1101(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6138.53(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    13833
_cell_measurement_theta_min      2.7725
_cell_measurement_theta_max      32.5022

_exptl_crystal_description       prisms
_exptl_crystal_colour            'Dark green'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2680
_exptl_absorpt_coefficient_mu    0.671
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_process_details   
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24583
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         32.59
_reflns_number_total             9890
_reflns_number_gt                7669
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0579P)²+0.5914P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9890
_refine_ls_number_parameters     373
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.1003
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr Cr 0.274728(11) 0.513015(14) 0.345551(10) 0.01671(6) Uani 1 1 d . . .
Cl1 Cl 0.18907(2) 0.52182(3) 0.269902(18) 0.02824(9) Uani 1 1 d . . .
Cl2 Cl 0.35034(2) 0.61545(2) 0.298339(16) 0.02513(8) Uani 1 1 d . . .
Cl3 Cl 0.21347(2) 0.62406(2) 0.398706(17) 0.02692(9) Uani 1 1 d . . .
N1 N 0.33699(6) 0.49704(8) 0.41794(6) 0.0207(2) Uani 1 1 d . . .
C2 C 0.38589(8) 0.55026(10) 0.45052(7) 0.0228(3) Uani 1 1 d . . .
C3 C 0.42670(8) 0.62644(10) 0.43648(7) 0.0264(3) Uani 1 1 d . . .
H3A H 0.4249 0.6520 0.3987 0.032 Uiso 1 1 calc R . .
C4 C 0.47134(8) 0.66565(11) 0.47988(8) 0.0301(3) Uani 1 1 d . . .
C5 C 0.51605(9) 0.74368(12) 0.46803(9) 0.0381(4) Uani 1 1 d . . .
H5A H 0.5164 0.7694 0.4302 0.046 Uiso 1 1 calc R . .
C6 C 0.55867(10) 0.78219(14) 0.51067(10) 0.0462(5) Uani 1 1 d . . .
H6A H 0.5878 0.8346 0.5023 0.055 Uiso 1 1 calc R . .
C7 C 0.55934(10) 0.74434(15) 0.56662(10) 0.0468(5) Uani 1 1 d . . .
H7A H 0.5888 0.7718 0.5958 0.056 Uiso 1 1 calc R . .
C8 C 0.51857(10) 0.66918(14) 0.57957(9) 0.0413(4) Uani 1 1 d . . .
H8A H 0.5202 0.6444 0.6176 0.050 Uiso 1 1 calc R . .
C9 C 0.47321(9) 0.62681(12) 0.53683(8) 0.0319(4) Uani 1 1 d . . .
C10 C 0.43133(9) 0.54865(12) 0.55017(7) 0.0319(3) Uani 1 1 d . . .
H10A H 0.4325 0.5220 0.5877 0.038 Uiso 1 1 calc R . .
C11 C 0.38884(8) 0.51239(10) 0.50710(7) 0.0264(3) Uani 1 1 d . . .
N12 N 0.34121(8) 0.43809(9) 0.50670(6) 0.0273(3) Uani 1 1 d D . .
H12 H 0.3299(12) 0.4051(14) 0.5384(6) 0.056(7) Uiso 1 1 d D . .
C13 C 0.31212(8) 0.43308(9) 0.45362(7) 0.0224(3) Uani 1 1 d . . .
C14 C 0.25769(9) 0.36386(10) 0.43452(6) 0.0241(3) Uani 1 1 d . . .
H14A H 0.2241 0.3492 0.4669 0.029 Uiso 1 1 calc R . .
H14B H 0.2832 0.3067 0.4230 0.029 Uiso 1 1 calc R . .
N15 N 0.21455(6) 0.40026(8) 0.38431(5) 0.0198(2) Uani 1 1 d . . .
C16 C 0.20962(8) 0.32733(10) 0.33907(7) 0.0221(3) Uani 1 1 d . . .
H16A H 0.1982 0.2672 0.3569 0.026 Uiso 1 1 calc R . .
H16B H 0.1707 0.3423 0.3108 0.026 Uiso 1 1 calc R . .
C17 C 0.28222(8) 0.32424(9) 0.31012(6) 0.0194(3) Uani 1 1 d . . .
N18 N 0.31422(7) 0.25245(8) 0.28413(6) 0.0242(3) Uani 1 1 d D . .
H18 H 0.2978(11) 0.1946(5) 0.2885(9) 0.044(6) Uiso 1 1 d D . .
C19 C 0.38326(8) 0.28059(10) 0.26574(7) 0.0249(3) Uani 1 1 d . . .
C20 C 0.43933(10) 0.23446(12) 0.23789(8) 0.0380(4) Uani 1 1 d . . .
H20A H 0.4343 0.1723 0.2261 0.046 Uiso 1 1 calc R . .
C21 C 0.50308(11) 0.28331(13) 0.22810(9) 0.0421(5) Uani 1 1 d . . .
H21A H 0.5428 0.2540 0.2089 0.051 Uiso 1 1 calc R . .
C22 C 0.51064(10) 0.37463(13) 0.24568(9) 0.0371(4) Uani 1 1 d . . .
H22A H 0.5558 0.4054 0.2391 0.045 Uiso 1 1 calc R . .
C23 C 0.45381(8) 0.42138(11) 0.27248(7) 0.0277(3) Uani 1 1 d . . .
H23A H 0.4589 0.4838 0.2838 0.033 Uiso 1 1 calc R . .
C24 C 0.38908(8) 0.37336(9) 0.28216(6) 0.0211(3) Uani 1 1 d . . .
N25 N 0.32372(6) 0.39898(8) 0.30914(5) 0.0188(2) Uani 1 1 d . . .
C26 C 0.13857(8) 0.42344(11) 0.40325(8) 0.0301(3) Uani 1 1 d . . .
H26A H 0.1154 0.3689 0.4201 0.045 Uiso 1 1 calc R . .
H26B H 0.1100 0.4442 0.3698 0.045 Uiso 1 1 calc R . .
H26C H 0.1404 0.4724 0.4323 0.045 Uiso 1 1 calc R . .
O30 O 0.32164(11) 0.34140(15) 0.60601(7) 0.0741(6) Uani 1 1 d . . .
C30 C 0.27377(14) 0.30718(19) 0.63622(10) 0.0595(7) Uani 1 1 d . . .
H30A H 0.2658 0.3345 0.6730 0.071 Uiso 1 1 calc R . .
N31 N 0.23239(11) 0.23669(14) 0.62298(8) 0.0542(5) Uani 1 1 d . . .
C32 C 0.23844(17) 0.19315(19) 0.56613(12) 0.0693(7) Uani 1 1 d . . .
H32A H 0.1940 0.2056 0.5436 0.104 Uiso 1 1 calc R . .
H32B H 0.2442 0.1267 0.5710 0.104 Uiso 1 1 calc R . .
H32C H 0.2811 0.2180 0.5457 0.104 Uiso 1 1 calc R . .
C33 C 0.17556(16) 0.2027(2) 0.66235(12) 0.0734(8) Uani 1 1 d . . .
H33A H 0.1749 0.2404 0.6975 0.110 Uiso 1 1 calc R . .
H33B H 0.1861 0.1387 0.6727 0.110 Uiso 1 1 calc R . .
H33C H 0.1277 0.2061 0.6432 0.110 Uiso 1 1 calc R . .
O40 O 0.16882(13) 0.4218(2) 0.54227(9) 0.1118(9) Uani 1 1 d . . .
C40 C 0.11677(16) 0.4038(2) 0.57246(11) 0.0788(9) Uani 1 1 d . . .
H40A H 0.0848 0.3565 0.5596 0.095 Uiso 1 1 calc R . .
N41 N 0.10077(13) 0.44421(16) 0.62170(9) 0.0652(6) Uani 1 1 d . . .
C42 C 0.1494(2) 0.5131(2) 0.64760(15) 0.1002(13) Uani 1 1 d . . .
H42A H 0.1965 0.5130 0.6272 0.150 Uiso 1 1 calc R . .
H42B H 0.1574 0.4983 0.6885 0.150 Uiso 1 1 calc R . .
H42C H 0.1269 0.5740 0.6444 0.150 Uiso 1 1 calc R . .
C43 C 0.03777(16) 0.4149(2) 0.65614(12) 0.0794(9) Uani 1 1 d . . .
H43A H 0.0033 0.4661 0.6602 0.119 Uiso 1 1 calc R . .
H43B H 0.0545 0.3954 0.6945 0.119 Uiso 1 1 calc R . .
H43C H 0.0133 0.3634 0.6368 0.119 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr N1 2.0354(13) . ?
Cr N25 2.0650(11) . ?
Cr N15 2.1687(12) . ?
Cr Cl2 2.3060(4) . ?
Cr Cl3 2.3178(4) . ?
Cr Cl1 2.3482(4) . ?
N1 C13 1.3240(19) . ?
N1 C2 1.4011(18) . ?
C2 C3 1.375(2) . ?
C2 C11 1.420(2) . ?
C3 C4 1.413(2) . ?
C4 C5 1.425(2) . ?
C4 C9 1.433(3) . ?
C5 C6 1.375(3) . ?
C6 C7 1.406(3) . ?
C7 C8 1.357(3) . ?
C8 C9 1.429(2) . ?
C9 C10 1.405(3) . ?
C10 C11 1.368(2) . ?
C11 N12 1.388(2) . ?
N12 C13 1.339(2) . ?
C13 C14 1.482(2) . ?
C14 N15 1.4986(19) . ?
N15 C26 1.4921(18) . ?
N15 C16 1.4930(18) . ?
C16 C17 1.484(2) . ?
C17 N25 1.3259(17) . ?
C17 N18 1.3395(18) . ?
N18 C19 1.391(2) . ?
C19 C20 1.383(2) . ?
C19 C24 1.407(2) . ?
C20 C21 1.382(3) . ?
C21 C22 1.397(3) . ?
C22 C23 1.386(2) . ?
C23 C24 1.391(2) . ?
C24 N25 1.3962(18) . ?
O30 C30 1.224(3) . ?
C30 N31 1.310(3) . ?
N31 C32 1.463(3) . ?
N31 C33 1.466(3) . ?
O40 C40 1.207(3) . ?
C40 N41 1.314(3) . ?
N41 C43 1.462(3) . ?
N41 C42 1.467(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
_geom_angle_publ_flag
N1 Cr N25 90.09(5) . . ?
N1 Cr N15 81.74(5) . . ?
N25 Cr N15 77.20(5) . . ?
N1 Cr Cl2 97.42(4) . . ?
N25 Cr Cl2 93.93(3) . . ?
N15 Cr Cl2 171.07(3) . . ?
N1 Cr Cl3 85.02(4) . . ?
N25 Cr Cl3 170.27(4) . . ?
N15 Cr Cl3 93.74(3) . . ?
Cl2 Cr Cl3 95.041(15) . . ?
N1 Cr Cl1 171.67(4) . . ?
N25 Cr Cl1 91.63(4) . . ?
N15 Cr Cl1 90.69(3) . . ?
Cl2 Cr Cl1 90.597(16) . . ?
Cl3 Cr Cl1 92.046(16) . . ?
C13 N1 C2 105.82(13) . . ?
C13 N1 Cr 113.64(10) . . ?
C2 N1 Cr 137.19(10) . . ?
C3 C2 N1 131.63(14) . . ?
C3 C2 C11 120.67(14) . . ?
N1 C2 C11 107.71(13) . . ?
C2 C3 C4 118.08(15) . . ?
C3 C4 C5 121.04(17) . . ?
C3 C4 C9 120.42(15) . . ?
C5 C4 C9 118.53(16) . . ?
C6 C5 C4 120.7(2) . . ?
C5 C6 C7 120.29(19) . . ?
C8 C7 C6 120.96(18) . . ?
C7 C8 C9 120.9(2) . . ?
C10 C9 C8 120.87(17) . . ?
C10 C9 C4 120.56(15) . . ?
C8 C9 C4 118.57(17) . . ?
C11 C10 C9 117.47(16) . . ?
C10 C11 N12 131.36(16) . . ?
C10 C11 C2 122.80(15) . . ?
N12 C11 C2 105.83(13) . . ?
C13 N12 C11 107.27(13) . . ?
N1 C13 N12 113.36(13) . . ?
N1 C13 C14 121.50(13) . . ?
N12 C13 C14 125.14(14) . . ?
C13 C14 N15 109.99(11) . . ?
C26 N15 C16 108.08(11) . . ?
C26 N15 C14 109.92(12) . . ?
C16 N15 C14 108.80(11) . . ?
C26 N15 Cr 114.83(9) . . ?
C16 N15 Cr 106.24(8) . . ?
C14 N15 Cr 108.77(8) . . ?
C17 C16 N15 106.47(11) . . ?
N25 C17 N18 112.59(12) . . ?
N25 C17 C16 119.48(12) . . ?
N18 C17 C16 127.92(12) . . ?
C17 N18 C19 107.56(12) . . ?
C20 C19 N18 131.99(14) . . ?
C20 C19 C24 122.42(15) . . ?
N18 C19 C24 105.59(12) . . ?
C21 C20 C19 116.67(16) . . ?
C20 C21 C22 121.68(16) . . ?
C23 C22 C21 121.57(16) . . ?
C22 C23 C24 117.39(15) . . ?
C23 C24 N25 131.50(13) . . ?
C23 C24 C19 120.23(13) . . ?
N25 C24 C19 108.21(12) . . ?
C17 N25 C24 106.01(11) . . ?
C17 N25 Cr 113.95(9) . . ?
C24 N25 Cr 140.03(9) . . ?
O30 C30 N31 126.6(3) . . ?
C30 N31 C32 120.4(2) . . ?
C30 N31 C33 121.8(2) . . ?
C32 N31 C33 117.7(2) . . ?
O40 C40 N41 125.3(3) . . ?
C40 N41 C43 121.0(3) . . ?
C40 N41 C42 121.7(3) . . ?
C43 N41 C42 117.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.884
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.063
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Cr-11-Cl3
_database_code_depnum_ccdc_archive 'CCDC 1473102'
_audit_update_record             
;
2016-04-08 deposited with the CCDC.
2018-01-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H19 Cl3 Cr N5, 2(C3 H7 N O)'
_chemical_formula_sum            'C25 H33 Cl3 Cr N7 O2'
_chemical_formula_weight         621.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.3091(3)
_cell_length_b                   11.3311(2)
_cell_length_c                   13.9361(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.1628(16)
_cell_angle_gamma                90.00
_cell_volume                     2845.85(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4404
_cell_measurement_theta_min      2.4497
_cell_measurement_theta_max      72.3091

_exptl_crystal_description       needles
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1292
_exptl_absorpt_coefficient_mu    6.200
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_process_details   
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) 
(compiled Apr 28 2010,14:27:37) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.2556
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10271
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         72.46
_reflns_number_total             5413
_reflns_number_gt                4230
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0124P)²+9.2480P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5413
_refine_ls_number_parameters     396
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1294
_refine_ls_wR_factor_gt          0.1251
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.150
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr Cr 0.15712(4) 0.26423(8) 0.78181(5) 0.0320(2) Uani 1 1 d . . .
Cl1 Cl 0.10480(7) 0.43400(11) 0.83964(7) 0.0402(3) Uani 1 1 d . . .
Cl2 Cl 0.23965(6) 0.23874(13) 0.92461(7) 0.0434(3) Uani 1 1 d . . .
Cl3 Cl 0.06969(6) 0.13691(11) 0.82964(7) 0.0361(3) Uani 1 1 d . . .
N1 N 0.19618(19) 0.1287(4) 0.7058(2) 0.0363(9) Uani 1 1 d D A .
C2 C 0.2546(3) 0.0494(4) 0.7144(3) 0.0355(11) Uani 1 1 d . . .
C3 C 0.3100(3) 0.0205(5) 0.7929(4) 0.0467(13) Uani 1 1 d . . .
H3A H 0.3135 0.0597 0.8538 0.056 Uiso 1 1 calc R . .
C4 C 0.3591(3) -0.0658(5) 0.7797(5) 0.0613(16) Uani 1 1 d . . .
H4A H 0.3970 -0.0870 0.8326 0.074 Uiso 1 1 calc R . .
C5 C 0.3553(3) -0.1243(5) 0.6901(5) 0.0583(15) Uani 1 1 d . . .
H5A H 0.3904 -0.1843 0.6839 0.070 Uiso 1 1 calc R . .
C6 C 0.3015(3) -0.0966(5) 0.6107(4) 0.0482(13) Uani 1 1 d . . .
H6A H 0.2989 -0.1351 0.5496 0.058 Uiso 1 1 calc R . .
C7 C 0.2517(3) -0.0094(5) 0.6251(3) 0.0381(11) Uani 1 1 d . . .
N8 N 0.1904(2) 0.0376(4) 0.5641(3) 0.0443(11) Uani 1 1 d D A .
H8 H 0.173(3) 0.016(5) 0.5020(14) 0.062(18) Uiso 1 1 d D . .
C9 C 0.1604(3) 0.1184(5) 0.6146(3) 0.0422(12) Uani 1 1 d D . .
C10 C 0.0977(4) 0.2062(7) 0.5706(4) 0.0331(17) Uani 0.668(7) 1 d PDU A 1
H10A H 0.1096 0.2450 0.5109 0.040 Uiso 0.668(7) 1 calc PR A 1
C11 C 0.0230(3) 0.1412(7) 0.5475(5) 0.0397(18) Uani 0.668(7) 1 d PDU A 1
H11A H 0.0161 0.1032 0.4826 0.048 Uiso 0.668(7) 1 calc PR A 1
H11B H 0.0186 0.0807 0.5975 0.048 Uiso 0.668(7) 1 calc PR A 1
C12 C -0.0317(4) 0.2411(8) 0.5498(5) 0.047(2) Uani 0.668(7) 1 d PDU A 1
H12A H -0.0815 0.2111 0.5561 0.057 Uiso 0.668(7) 1 calc PR A 1
H12B H -0.0360 0.2912 0.4909 0.057 Uiso 0.668(7) 1 calc PR A 1
C10' C 0.1154(6) 0.3682(12) 0.5809(10) 0.027(3) Uiso 0.332(7) 1 d PDU A 2
H10B H 0.1220 0.3284 0.5190 0.033 Uiso 0.332(7) 1 calc PR A 2
C11' C 0.0558(6) 0.4627(10) 0.5617(10) 0.038(3) Uiso 0.332(7) 1 d PDU A 2
H11C H 0.0572 0.5047 0.4998 0.046 Uiso 0.332(7) 1 calc PR A 2
H11D H 0.0611 0.5207 0.6157 0.046 Uiso 0.332(7) 1 calc PR A 2
C12' C -0.0155(6) 0.3908(12) 0.5558(9) 0.040(4) Uiso 0.332(7) 1 d PDU A 2
H12C H -0.0581 0.4417 0.5636 0.048 Uiso 0.332(7) 1 calc PR A 2
H12D H -0.0274 0.3475 0.4933 0.048 Uiso 0.332(7) 1 calc PR A 2
C13 C 0.0044(2) 0.3073(4) 0.6408(3) 0.0344(11) Uani 1 1 d D . .
H13A H -0.0096 0.3917 0.6368 0.041 Uiso 0.668(7) 1 calc PR A 1
H13B H -0.0098 0.2726 0.7001 0.041 Uiso 0.668(7) 1 calc PR A 1
H13C H -0.0228 0.2346 0.6309 0.041 Uiso 0.332(7) 1 d PR A 2
H13D H -0.0037 0.3434 0.7003 0.041 Uiso 0.332(7) 1 d PR A 2
N14 N 0.0864(2) 0.2917(4) 0.6410(3) 0.0415(11) Uani 1 1 d D A .
C15 C 0.1108(4) 0.4212(7) 0.6069(5) 0.0360(17) Uani 0.668(7) 1 d PDU A 1
H15A H 0.0961 0.4313 0.5355 0.043 Uiso 0.668(7) 1 calc PR A 1
H15B H 0.0879 0.4847 0.6402 0.043 Uiso 0.668(7) 1 calc PR A 1
C15' C 0.0830(6) 0.1558(12) 0.5892(10) 0.031(4) Uiso 0.332(7) 1 d PDU A 2
H15C H 0.0497 0.1023 0.6174 0.037 Uiso 0.332(7) 1 calc PR A 2
H15D H 0.0667 0.1600 0.5177 0.037 Uiso 0.332(7) 1 calc PR A 2
C16 C 0.1917(3) 0.4221(5) 0.6357(3) 0.0402(12) Uani 1 1 d D . .
N17 N 0.2378(2) 0.4895(4) 0.5946(3) 0.0369(9) Uani 1 1 d D A .
H17 H 0.224(3) 0.523(4) 0.5358(17) 0.044(15) Uiso 1 1 d D . .
C18 C 0.3074(3) 0.4792(5) 0.6506(3) 0.0382(11) Uani 1 1 d . . .
C19 C 0.3747(3) 0.5279(6) 0.6403(4) 0.0535(15) Uani 1 1 d . A .
H19A H 0.3790 0.5810 0.5889 0.064 Uiso 1 1 calc R . .
C20 C 0.4350(3) 0.4958(7) 0.7085(5) 0.074(2) Uani 1 1 d . . .
H20A H 0.4825 0.5266 0.7034 0.089 Uiso 1 1 calc R A .
C21 C 0.4288(3) 0.4198(7) 0.7841(5) 0.0667(18) Uani 1 1 d . A .
H21A H 0.4721 0.4001 0.8296 0.080 Uiso 1 1 calc R . .
C22 C 0.3613(3) 0.3710(5) 0.7962(4) 0.0470(13) Uani 1 1 d . . .
H22A H 0.3574 0.3190 0.8485 0.056 Uiso 1 1 calc R A .
C23 C 0.2999(2) 0.4026(4) 0.7273(3) 0.0332(10) Uani 1 1 d . A .
N24 N 0.2258(2) 0.3689(4) 0.7163(2) 0.0344(9) Uani 1 1 d D A .
O30 O 0.2169(2) 0.6440(4) 0.4444(3) 0.0544(10) Uani 1 1 d . . .
C30 C 0.1820(3) 0.6420(5) 0.3607(4) 0.0439(12) Uani 1 1 d . . .
H30A H 0.1495 0.5775 0.3418 0.053 Uiso 1 1 calc R . .
N31 N 0.1872(2) 0.7250(4) 0.2949(3) 0.0460(11) Uani 1 1 d . . .
C32 C 0.2399(4) 0.8211(5) 0.3160(4) 0.0617(16) Uani 1 1 d . . .
H32A H 0.2137 0.8932 0.3290 0.093 Uiso 1 1 calc R . .
H32B H 0.2646 0.8339 0.2600 0.093 Uiso 1 1 calc R . .
H32C H 0.2770 0.8012 0.3734 0.093 Uiso 1 1 calc R . .
C33 C 0.1379(4) 0.7239(7) 0.2002(4) 0.073(2) Uani 1 1 d . . .
H33A H 0.1129 0.6472 0.1903 0.110 Uiso 1 1 calc R . .
H33B H 0.1670 0.7371 0.1485 0.110 Uiso 1 1 calc R . .
H33C H 0.1008 0.7865 0.1982 0.110 Uiso 1 1 calc R . .
O40 O 0.4123(5) 0.7383(9) 1.0019(7) 0.083(3) Uani 0.533(10) 1 d PDU B 1
C40 C 0.4581(5) 0.6981(11) 0.9548(10) 0.056(3) Uani 0.533(10) 1 d PDU B 1
H40A H 0.4446 0.6316 0.9140 0.068 Uiso 0.533(10) 1 calc PR B 1
N41 N 0.5263(4) 0.7448(10) 0.9591(7) 0.046(2) Uani 0.533(10) 1 d PDU B 1
C42 C 0.5473(8) 0.8532(12) 1.0148(10) 0.069(4) Uani 0.533(10) 1 d PDU B 1
H42A H 0.5127 0.9166 0.9898 0.103 Uiso 0.533(10) 1 calc PR B 1
H42B H 0.5977 0.8761 1.0080 0.103 Uiso 0.533(10) 1 calc PR B 1
H42C H 0.5454 0.8394 1.0837 0.103 Uiso 0.533(10) 1 calc PR B 1
C43 C 0.5788(6) 0.6906(12) 0.9012(9) 0.056(3) Uani 0.533(10) 1 d PDU B 1
H43A H 0.6223 0.6603 0.9455 0.084 Uiso 0.533(10) 1 calc PR B 1
H43B H 0.5944 0.7502 0.8581 0.084 Uiso 0.533(10) 1 calc PR B 1
H43C H 0.5540 0.6255 0.8620 0.084 Uiso 0.533(10) 1 calc PR B 1
O40' O 0.4984(7) 0.8554(10) 1.0464(9) 0.090(4) Uiso 0.467(10) 1 d PDU B 2
C40' C 0.5438(8) 0.8031(11) 1.0053(12) 0.049(4) Uiso 0.467(10) 1 d PDU B 2
H40B H 0.5925 0.8341 1.0100 0.059 Uiso 0.467(10) 1 calc PR B 2
N41' N 0.5255(6) 0.7035(10) 0.9543(9) 0.039(3) Uiso 0.467(10) 1 d PDU B 2
C42' C 0.4509(8) 0.6535(18) 0.9408(16) 0.079(6) Uiso 0.467(10) 1 d PDU B 2
H42D H 0.4238 0.6876 0.9888 0.119 Uiso 0.467(10) 1 calc PR B 2
H42E H 0.4542 0.5677 0.9496 0.119 Uiso 0.467(10) 1 calc PR B 2
H42F H 0.4246 0.6715 0.8749 0.119 Uiso 0.467(10) 1 calc PR B 2
C43' C 0.5829(9) 0.6396(15) 0.9103(13) 0.074(5) Uiso 0.467(10) 1 d PDU B 2
H43D H 0.5690 0.6406 0.8391 0.111 Uiso 0.467(10) 1 calc PR B 2
H43E H 0.5863 0.5578 0.9334 0.111 Uiso 0.467(10) 1 calc PR B 2
H43F H 0.6310 0.6785 0.9297 0.111 Uiso 0.467(10) 1 calc PR B 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr N24 2.055(4) . ?
Cr N1 2.064(4) . ?
Cr N14 2.175(4) . ?
Cr Cl2 2.2948(12) . ?
Cr Cl3 2.3376(13) . ?
Cr Cl1 2.3538(15) . ?
N1 C9 1.328(5) . ?
N1 C2 1.386(6) . ?
C2 C3 1.393(6) . ?
C2 C7 1.404(7) . ?
C3 C4 1.362(8) . ?
C4 C5 1.405(8) . ?
C5 C6 1.381(8) . ?
C6 C7 1.384(7) . ?
C7 N8 1.388(6) . ?
N8 C9 1.331(6) . ?
C9 C15' 1.462(11) . ?
C9 C10 1.561(8) . ?
C10 N14 1.419(8) . ?
C10 C11 1.536(9) . ?
C11 C12 1.516(10) . ?
C12 C13 1.520(8) . ?
C10' N14 1.375(13) . ?
C10' C11' 1.519(14) . ?
C10' C16 1.590(11) . ?
C11' C12' 1.529(14) . ?
C12' C13 1.510(12) . ?
C13 N14 1.512(5) . ?
N14 C15 1.628(8) . ?
N14 C15' 1.697(12) . ?
C15 C16 1.465(8) . ?
C16 N24 1.329(6) . ?
C16 N17 1.340(6) . ?
N17 C18 1.377(6) . ?
C18 C19 1.380(7) . ?
C18 C23 1.403(6) . ?
C19 C20 1.373(8) . ?
C20 C21 1.382(9) . ?
C21 C22 1.390(7) . ?
C22 C23 1.389(7) . ?
C23 N24 1.392(6) . ?
O30 C30 1.228(6) . ?
C30 N31 1.329(6) . ?
N31 C32 1.449(7) . ?
N31 C33 1.462(7) . ?
O40 C40 1.240(8) . ?
C40 N41 1.348(8) . ?
N41 C42 1.467(8) . ?
N41 C43 1.492(8) . ?
O40' C40' 1.239(9) . ?
C40' N41' 1.345(8) . ?
N41' C42' 1.460(9) . ?
N41' C43' 1.494(9) . ?

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
_geom_angle_publ_flag
N24 Cr N1 84.66(16) . . ?
N24 Cr N14 80.20(14) . . ?
N1 Cr N14 81.27(15) . . ?
N24 Cr Cl2 95.56(10) . . ?
N1 Cr Cl2 96.71(11) . . ?
N14 Cr Cl2 175.44(11) . . ?
N24 Cr Cl3 170.38(11) . . ?
N1 Cr Cl3 90.22(11) . . ?
N14 Cr Cl3 90.99(11) . . ?
Cl2 Cr Cl3 93.11(5) . . ?
N24 Cr Cl1 89.90(12) . . ?
N1 Cr Cl1 169.33(11) . . ?
N14 Cr Cl1 88.78(12) . . ?
Cl2 Cr Cl1 92.95(5) . . ?
Cl3 Cr Cl1 93.80(5) . . ?
C9 N1 C2 105.6(4) . . ?
C9 N1 Cr 113.6(3) . . ?
C2 N1 Cr 140.3(3) . . ?
N1 C2 C3 131.7(5) . . ?
N1 C2 C7 108.8(4) . . ?
C3 C2 C7 119.5(5) . . ?
C4 C3 C2 118.0(5) . . ?
C3 C4 C5 121.9(5) . . ?
C6 C5 C4 121.4(5) . . ?
C5 C6 C7 116.2(5) . . ?
C6 C7 N8 131.8(5) . . ?
C6 C7 C2 123.0(5) . . ?
N8 C7 C2 105.2(4) . . ?
C9 N8 C7 107.7(4) . . ?
N1 C9 N8 112.7(4) . . ?
N1 C9 C15' 120.0(6) . . ?
N8 C9 C15' 123.0(6) . . ?
N1 C9 C10 121.6(5) . . ?
N8 C9 C10 125.1(4) . . ?
N14 C10 C11 103.9(5) . . ?
N14 C10 C9 110.5(4) . . ?
C11 C10 C9 110.1(6) . . ?
C12 C11 C10 101.8(6) . . ?
C11 C12 C13 101.2(5) . . ?
N14 C10' C11' 102.0(8) . . ?
N14 C10' C16 110.5(8) . . ?
C11' C10' C16 110.9(10) . . ?
C10' C11' C12' 102.4(9) . . ?
C13 C12' C11' 101.9(8) . . ?
C12' C13 N14 100.2(5) . . ?
C12' C13 C12 69.3(7) . . ?
N14 C13 C12 103.3(4) . . ?
C10' N14 C13 114.6(5) . . ?
C10 N14 C13 110.1(4) . . ?
C10 N14 C15 109.5(5) . . ?
C13 N14 C15 102.6(4) . . ?
C10' N14 C15' 107.6(8) . . ?
C13 N14 C15' 98.2(5) . . ?
C10' N14 Cr 114.0(5) . . ?
C10 N14 Cr 112.9(3) . . ?
C13 N14 Cr 116.8(2) . . ?
C15 N14 Cr 104.0(3) . . ?
C15' N14 Cr 103.0(5) . . ?
C16 C15 N14 104.0(5) . . ?
C9 C15' N14 101.5(8) . . ?
N24 C16 N17 112.5(4) . . ?
N24 C16 C15 122.0(4) . . ?
N17 C16 C15 124.7(5) . . ?
N24 C16 C10' 118.2(6) . . ?
N17 C16 C10' 125.4(6) . . ?
C16 N17 C18 107.4(4) . . ?
N17 C18 C19 131.4(5) . . ?
N17 C18 C23 106.2(4) . . ?
C19 C18 C23 122.3(5) . . ?
C20 C19 C18 116.5(5) . . ?
C19 C20 C21 121.9(5) . . ?
C20 C21 C22 122.3(6) . . ?
C23 C22 C21 116.2(5) . . ?
C22 C23 N24 131.3(4) . . ?
C22 C23 C18 120.7(4) . . ?
N24 C23 C18 108.0(4) . . ?
C16 N24 C23 105.8(4) . . ?
C16 N24 Cr 113.8(3) . . ?
C23 N24 Cr 140.4(3) . . ?
O30 C30 N31 123.6(6) . . ?
C30 N31 C32 121.2(5) . . ?
C30 N31 C33 120.6(5) . . ?
C32 N31 C33 118.2(5) . . ?
O40 C40 N41 122.7(10) . . ?
C40 N41 C42 120.5(8) . . ?
C40 N41 C43 119.6(8) . . ?
C42 N41 C43 119.8(8) . . ?
O40' C40' N41' 121.3(12) . . ?
C40' N41' C42' 122.3(10) . . ?
C40' N41' C43' 119.7(10) . . ?
C42' N41' C43' 118.0(10) . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        69.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.072

#===END



