# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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. 
# 
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data_publication_text
_database_code_depnum_ccdc_archive 'CCDC 1031521'
_audit_update_record             
;
2014-12-21 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_chemical_name_id                '[CrO2(tpenaH)](ClO4)2(H2O2)4'
_chemical_name_common            4

_chemical_melting_point          ?
_chemical_formula_sum            'C22 H33 Cl2 Cr N5 O19'
_chemical_formula_weight         794.42

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   15.2360(16)
_cell_length_b                   14.7664(16)
_cell_length_c                   16.0081(17)
_cell_angle_alpha                90
_cell_angle_beta                 118.237(5)
_cell_angle_gamma                90
_cell_volume                     3172.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             1647
_exptl_transmission_factor_min   0.5698
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.623
_shelx_estimated_absorpt_T_min   0.845
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS v2008/1 (Sheldrick, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed-tube'
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice ω and φ scans'
_diffrn_detector_area_resol_mean 9.1
_diffrn_reflns_number            43336
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.753
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.993

_reflns_number_total             6430
_reflns_number_gt                4722
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
Reflections were merged by SHELXL according to the crystal 
class for the calculation of statistics and refinement. 
 
_reflns_Friedel_fraction is defined as the number of unique 
Friedel pairs measured divided by the number that would be 
possible theoretically, ignoring centric projections and 
systematic absences. 
;

_computing_data_collection       'APEX2 v.2010.1-2 (Bruker Nonius, 2010)'
_computing_cell_refinement       'SAINT v.7.68a (Bruker, 2010)'
_computing_data_reduction        'SAINT v.7.68a (Bruker, 2010)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    
'Mercury 3.11 (Macrae at al., 2008) and POV-RAY (Cason, 2004)'
_computing_publication_material  'SHELX-2013 (Sheldrick, 2008)'
_refine_special_details          
; 
Hydrogen atoms connected to O13, O14 and O16 were located in electron difference density maps. Remaining hydrogen atoms associated with hydrogen peroxide were placed on calculated positions based on an as reasonable as possible bonding network. The O-O and O-H bond distances were restrained to 1.46 and 0.98 A respectively. The identities of O17 and O18 was difficult to determine. With an unrestrained bond distance of 1.35 A they did not match either H2O2 a co-crystallized O2 molecule or two coexisting water molecules. Finally they were modelled as partially occupied water molecules and refined with a free variable SOF summed to unity. 
The quality of the data is clearly poor. Data reduction and absorption correction were considered however no improvement was possible. The crystal was weakly diffracting requiring an exposure time of 120 seconds per frame with a total collection time of 72 hours. A second data collection was performed on a different crystal yielding the same overall quality. Out of at least 20 preparations only on a couple of occasions were crystals of suitable size, albeit weakly diffracting, of this unstable compound obtained. Decomposition of the crystal during the long data collection must be expected. At rt the crystal collapsed within hours.
;
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1406P)²+33.1301P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6430
_refine_ls_number_parameters     473
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.1030
_refine_ls_wR_factor_ref         0.3020
_refine_ls_wR_factor_gt          0.2841
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.053
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.62940(8) 0.54604(7) 0.31556(7) 0.0180(3) Uani 1 1 d . . . . .
Cl1 Cl 0.49055(13) 0.25326(12) 0.02462(14) 0.0323(5) Uani 1 1 d . . . . .
O1 O 0.7258(4) 0.7613(3) 0.2362(4) 0.0275(11) Uani 1 1 d . . . . .
N1 N 0.7719(5) 0.3671(4) 0.1234(4) 0.0242(12) Uani 1 1 d D . . . .
H1N H 0.782(6) 0.329(4) 0.172(4) 0.029 Uiso 1 1 d D U . . .
C1 C 0.8211(6) 0.3448(5) 0.0763(6) 0.0323(17) Uani 1 1 d . . . . .
H1A H 0.8673 0.2961 0.0982 0.039 Uiso 1 1 calc R U . . .
Cl2 Cl 0.23340(16) 0.61707(15) 0.27728(15) 0.0394(5) Uani 1 1 d . . . . .
O2 O 0.6694(4) 0.6686(3) 0.3081(3) 0.0222(10) Uani 1 1 d . . . . .
N2 N 0.7097(4) 0.5156(4) 0.2377(4) 0.0179(11) Uani 1 1 d . . . . .
C2 C 0.8055(7) 0.3919(5) -0.0041(6) 0.039(2) Uani 1 1 d . . . . .
H2 H 0.8415 0.3775 -0.0371 0.047 Uiso 1 1 calc R U . . .
O3 O 0.5236(4) 0.5427(4) 0.1906(4) 0.0342(13) Uani 1 1 d . . . . .
N3 N 0.7719(4) 0.5251(4) 0.4317(4) 0.0190(11) Uani 1 1 d . . . . .
C3 C 0.7357(8) 0.4605(6) -0.0347(6) 0.043(2) Uani 1 1 d . . . . .
H3 H 0.7220 0.4927 -0.0910 0.052 Uiso 1 1 calc R U . . .
O4 O 0.4920(4) 0.5721(4) 0.2544(4) 0.0363(13) Uani 1 1 d . . . . .
N4 N 0.6142(4) 0.4123(4) 0.3384(4) 0.0239(12) Uani 1 1 d . . . . .
C4 C 0.6862(6) 0.4829(5) 0.0142(5) 0.0334(18) Uani 1 1 d . . . . .
H4 H 0.6390 0.5308 -0.0073 0.040 Uiso 1 1 calc R U . . .
N5 N 0.6154(4) 0.5873(4) 0.4333(4) 0.0232(12) Uani 1 1 d . . . . .
O5 O 0.4761(10) 0.3361(7) -0.0173(9) 0.163(8) Uani 1 1 d . . . . .
C5 C 0.7049(5) 0.4355(4) 0.0953(5) 0.0249(15) Uani 1 1 d . . . . .
O6 O 0.4613(6) 0.1823(6) -0.0406(6) 0.077(3) Uani 1 1 d . . . . .
C6 C 0.6542(5) 0.4532(5) 0.1553(5) 0.0235(14) Uani 1 1 d . . . . .
H6A H 0.5875 0.4793 0.1143 0.028 Uiso 1 1 calc R U . . .
H6B H 0.6443 0.3945 0.1797 0.028 Uiso 1 1 calc R U . . .
O7 O 0.5900(5) 0.2465(4) 0.0949(6) 0.065(2) Uani 1 1 d . . . . .
C7 C 0.7251(6) 0.6053(4) 0.2027(5) 0.0229(14) Uani 1 1 d . . . . .
H7A H 0.6797 0.6097 0.1337 0.028 Uiso 1 1 calc R U . . .
H7B H 0.7943 0.6085 0.2127 0.028 Uiso 1 1 calc R U . . .
O8 O 0.4277(8) 0.2542(15) 0.0630(11) 0.182(9) Uani 1 1 d . . . . .
C8 C 0.7066(5) 0.6847(4) 0.2520(5) 0.0214(14) Uani 1 1 d . . . . .
O9 O 0.2851(6) 0.5434(5) 0.3344(6) 0.067(2) Uani 1 1 d . . . . .
C9 C 0.8062(5) 0.4730(4) 0.3060(5) 0.0208(14) Uani 1 1 d . . . . .
H9A H 0.8538 0.4750 0.2802 0.025 Uiso 1 1 calc R U . . .
H9B H 0.7955 0.4089 0.3169 0.025 Uiso 1 1 calc R U . . .
O10 O 0.1554(8) 0.5906(8) 0.1881(7) 0.099(3) Uani 1 1 d . . . . .
C10 C 0.8473(5) 0.5252(5) 0.3978(5) 0.0212(14) Uani 1 1 d . . . . .
H10A H 0.9097 0.4966 0.4457 0.025 Uiso 1 1 calc R U . . .
H10B H 0.8625 0.5881 0.3876 0.025 Uiso 1 1 calc R U . . .
O11 O 0.2967(6) 0.6732(6) 0.2600(7) 0.077(3) Uani 1 1 d . . . . .
C11 C 0.7711(5) 0.4358(5) 0.4780(5) 0.0252(15) Uani 1 1 d . . . . .
H11A H 0.8361 0.4053 0.4992 0.030 Uiso 1 1 calc R U . . .
H11B H 0.7630 0.4479 0.5348 0.030 Uiso 1 1 calc R U . . .
O12 O 0.1866(7) 0.6632(6) 0.3253(6) 0.073(2) Uani 1 1 d . . . . .
C12 C 0.6905(5) 0.3744(5) 0.4138(5) 0.0244(15) Uani 1 1 d . . . . .
C13 C 0.6911(7) 0.2831(5) 0.4347(6) 0.0337(18) Uani 1 1 d . . . . .
H13 H 0.7460 0.2573 0.4884 0.040 Uiso 1 1 calc R U . . .
O13 O -0.0396(6) 0.5232(6) 0.2146(6) 0.073(2) Uani 1 1 d D . . . .
H13O H -0.007(6) 0.465(3) 0.217(7) 0.05(3) Uiso 1 1 d D . . . .
C14 C 0.6116(7) 0.2314(5) 0.3767(7) 0.042(2) Uani 1 1 d . . . . .
H14 H 0.6103 0.1689 0.3900 0.050 Uiso 1 1 calc R U . . .
O14 O 0.0203(6) 0.5406(6) 0.3151(6) 0.074(2) Uani 1 1 d D . . . .
H14O H 0.065(6) 0.589(5) 0.317(7) 0.05(3) Uiso 1 1 d D . . . .
C15 C 0.5337(7) 0.2690(6) 0.2994(7) 0.042(2) Uani 1 1 d . . . . .
H15 H 0.4781 0.2328 0.2589 0.051 Uiso 1 1 calc R U . . .
H15O H 0.318(7) 0.439(5) 0.177(7) 0.051 Uiso 1 1 d D U . . .
O15 O 0.2867(9) 0.3964(6) 0.2018(6) 0.094(3) Uani 1 1 d D . . . .
C16 C 0.5357(6) 0.3600(5) 0.2801(6) 0.0320(17) Uani 1 1 d . . . . .
H16 H 0.4819 0.3861 0.2258 0.017(18) Uiso 1 1 calc R . . . .
H16O H 0.202(5) 0.327(5) 0.168(4) 0.020 Uiso 1 1 d D U . . .
O16 O 0.2238(10) 0.3406(7) 0.1209(7) 0.107(4) Uani 1 1 d D . . . .
C17 C 0.7915(5) 0.5998(5) 0.5005(5) 0.0254(15) Uani 1 1 d . . . . .
H17A H 0.8469 0.5831 0.5632 0.031 Uiso 1 1 calc R U . . .
H17B H 0.8106 0.6555 0.4785 0.031 Uiso 1 1 calc R U . . .
C18 C 0.6992(5) 0.6159(4) 0.5079(5) 0.0241(14) Uani 1 1 d . . . . .
C19 C 0.6976(6) 0.6618(6) 0.5832(6) 0.0334(17) Uani 1 1 d . . . . .
H19 H 0.7572 0.6854 0.6334 0.040 Uiso 1 1 calc R U . . .
H19O H 0.550(9) 0.130(10) 0.747(7) 0.08(4) Uiso 1 1 d D . . . .
O19 O 0.5788(10) 0.1170(9) 0.7041(10) 0.123(4) Uani 1 1 d D . . . .
C20 C 0.6084(7) 0.6724(6) 0.5832(6) 0.041(2) Uani 1 1 d . . . . .
H20 H 0.6057 0.7024 0.6345 0.049 Uiso 1 1 calc R U . . .
H20O H 0.608(4) 0.173(10) 0.627(10) 0.08(5) Uiso 1 1 d D . . . .
O20 O 0.5386(12) 0.1625(13) 0.6125(10) 0.159(6) Uani 1 1 d D . . . .
C21 C 0.5227(7) 0.6394(6) 0.5088(7) 0.042(2) Uani 1 1 d . . . . .
H21 H 0.4604 0.6460 0.5081 0.050 Uiso 1 1 calc R U . . .
C22 C 0.5287(6) 0.5971(5) 0.4355(6) 0.0323(17) Uani 1 1 d . . . . .
H22 H 0.4695 0.5737 0.3845 0.039 Uiso 1 1 calc R U . . .
O17 O 0.0667(6) 0.2522(6) 0.3200(7) 0.052(3) Uani 0.754(16) 1 d . . P A 1
O18 O -0.0113(12) 0.3103(12) 0.3017(12) 0.017(5) Uiso 0.246(16) 1 d . . P A 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
Cr1 O3 1.884(5) . ?
Cr1 O4 1.884(5) . ?
Cr1 O2 1.931(5) . ?
Cr1 N4 2.041(6) . ?
Cr1 N5 2.085(6) . ?
Cr1 N3 2.108(5) . ?
Cr1 N2 2.167(6) . ?
Cl1 O5 1.363(9) . ?
Cl1 O8 1.361(12) . ?
Cl1 O6 1.395(7) . ?
Cl1 O7 1.399(7) . ?
O1 C8 1.224(8) . ?
N1 C1 1.332(10) . ?
N1 C5 1.353(9) . ?
N1 H1N 0.907(10) . ?
C1 C2 1.381(11) . ?
C1 H1A 0.9500 . ?
Cl2 O9 1.399(7) . ?
Cl2 O11 1.396(8) . ?
Cl2 O10 1.414(10) . ?
Cl2 O12 1.443(8) . ?
O2 C8 1.290(8) . ?
N2 C9 1.494(8) . ?
N2 C7 1.499(8) . ?
N2 C6 1.500(8) . ?
C2 C3 1.380(13) . ?
C2 H2 0.9500 . ?
O3 O4 1.388(8) . ?
N3 C17 1.486(9) . ?
N3 C10 1.485(9) . ?
N3 C11 1.516(8) . ?
C3 C4 1.361(12) . ?
C3 H3 0.9500 . ?
N4 C12 1.339(9) . ?
N4 C16 1.357(9) . ?
C4 C5 1.380(11) . ?
C4 H4 0.9500 . ?
N5 C18 1.339(9) . ?
N5 C22 1.347(9) . ?
C5 C6 1.513(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.513(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 C10 1.507(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.481(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.388(10) . ?
C13 C14 1.360(13) . ?
C13 H13 0.9500 . ?
O13 O14 1.449(8) . ?
O13 H13O 0.982(10) . ?
C14 C15 1.363(14) . ?
C14 H14 0.9500 . ?
O14 H14O 0.980(10) . ?
C15 C16 1.383(12) . ?
C15 H15 0.9500 . ?
O15 O16 1.450(8) . ?
O15 H15O 0.982(10) . ?
C16 H16 0.9500 . ?
O16 H16O 0.985(10) . ?
C17 C18 1.486(10) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.393(10) . ?
C19 C20 1.368(12) . ?
C19 H19 0.9500 . ?
O19 O20 1.458(9) . ?
O19 H19O 0.982(10) . ?
C20 C21 1.375(13) . ?
C20 H20 0.9500 . ?
O20 H20O 0.986(10) . ?
C21 C22 1.369(12) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?

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
O3 Cr1 O4 43.2(2) . . ?
O3 Cr1 O2 95.5(2) . . ?
O4 Cr1 O2 94.7(2) . . ?
O3 Cr1 N4 93.0(3) . . ?
O4 Cr1 N4 95.7(3) . . ?
O2 Cr1 N4 169.5(2) . . ?
O3 Cr1 N5 124.4(2) . . ?
O4 Cr1 N5 81.2(2) . . ?
O2 Cr1 N5 87.3(2) . . ?
N4 Cr1 N5 93.0(2) . . ?
O3 Cr1 N3 159.9(2) . . ?
O4 Cr1 N3 156.3(2) . . ?
O2 Cr1 N3 88.2(2) . . ?
N4 Cr1 N3 81.8(2) . . ?
N5 Cr1 N3 75.5(2) . . ?
O3 Cr1 N2 79.4(2) . . ?
O4 Cr1 N2 122.3(2) . . ?
O2 Cr1 N2 83.0(2) . . ?
N4 Cr1 N2 92.6(2) . . ?
N5 Cr1 N2 155.2(2) . . ?
N3 Cr1 N2 81.4(2) . . ?
O5 Cl1 O8 103.3(13) . . ?
O5 Cl1 O6 112.7(7) . . ?
O8 Cl1 O6 107.5(7) . . ?
O5 Cl1 O7 108.8(6) . . ?
O8 Cl1 O7 111.3(8) . . ?
O6 Cl1 O7 112.9(5) . . ?
C1 N1 C5 122.3(6) . . ?
C1 N1 H1N 115(5) . . ?
C5 N1 H1N 123(5) . . ?
N1 C1 C2 120.5(7) . . ?
N1 C1 H1A 119.7 . . ?
C2 C1 H1A 119.7 . . ?
O9 Cl2 O11 111.3(5) . . ?
O9 Cl2 O10 112.9(7) . . ?
O11 Cl2 O10 107.1(6) . . ?
O9 Cl2 O12 106.6(5) . . ?
O11 Cl2 O12 112.8(6) . . ?
O10 Cl2 O12 106.1(6) . . ?
C8 O2 Cr1 118.1(4) . . ?
C9 N2 C7 111.8(5) . . ?
C9 N2 C6 109.6(5) . . ?
C7 N2 C6 109.7(5) . . ?
C9 N2 Cr1 107.1(4) . . ?
C7 N2 Cr1 105.2(4) . . ?
C6 N2 Cr1 113.4(4) . . ?
C3 C2 C1 117.8(8) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
O4 O3 Cr1 68.4(3) . . ?
C17 N3 C10 110.6(5) . . ?
C17 N3 C11 109.2(5) . . ?
C10 N3 C11 111.5(5) . . ?
C17 N3 Cr1 107.9(4) . . ?
C10 N3 Cr1 109.3(4) . . ?
C11 N3 Cr1 108.4(4) . . ?
C4 C3 C2 121.1(8) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
O3 O4 Cr1 68.4(3) . . ?
C12 N4 C16 119.3(7) . . ?
C12 N4 Cr1 116.2(5) . . ?
C16 N4 Cr1 124.4(5) . . ?
C3 C4 C5 119.7(7) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C18 N5 C22 118.4(6) . . ?
C18 N5 Cr1 115.9(5) . . ?
C22 N5 Cr1 125.2(5) . . ?
N1 C5 C4 118.6(7) . . ?
N1 C5 C6 116.7(6) . . ?
C4 C5 C6 124.7(7) . . ?
N2 C6 C5 114.8(5) . . ?
N2 C6 H6A 108.6 . . ?
C5 C6 H6A 108.6 . . ?
N2 C6 H6B 108.6 . . ?
C5 C6 H6B 108.6 . . ?
H6A C6 H6B 107.5 . . ?
N2 C7 C8 112.9(5) . . ?
N2 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
N2 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
O1 C8 O2 122.8(6) . . ?
O1 C8 C7 119.1(6) . . ?
O2 C8 C7 118.2(6) . . ?
N2 C9 C10 108.1(5) . . ?
N2 C9 H9A 110.1 . . ?
C10 C9 H9A 110.1 . . ?
N2 C9 H9B 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N3 C10 C9 108.6(5) . . ?
N3 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
N3 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.3 . . ?
C12 C11 N3 112.9(6) . . ?
C12 C11 H11A 109.0 . . ?
N3 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
N3 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N4 C12 C13 121.8(7) . . ?
N4 C12 C11 116.8(6) . . ?
C13 C12 C11 121.2(7) . . ?
C14 C13 C12 118.6(8) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
O14 O13 H13O 94(6) . . ?
C15 C14 C13 120.2(8) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
O13 O14 H14O 103(6) . . ?
C14 C15 C16 119.7(8) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
O16 O15 H15O 105(6) . . ?
N4 C16 C15 120.4(8) . . ?
N4 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
O15 O16 H16O 75(5) . . ?
C18 C17 N3 108.2(5) . . ?
C18 C17 H17A 110.1 . . ?
N3 C17 H17A 110.1 . . ?
C18 C17 H17B 110.1 . . ?
N3 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
N5 C18 C19 121.7(7) . . ?
N5 C18 C17 114.7(6) . . ?
C19 C18 C17 123.5(7) . . ?
C20 C19 C18 118.7(8) . . ?
C20 C19 H19 120.6 . . ?
C18 C19 H19 120.6 . . ?
O20 O19 H19O 120(8) . . ?
C21 C20 C19 119.6(8) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
O19 O20 H20O 87(8) . . ?
C22 C21 C20 119.0(8) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
N5 C22 C21 122.4(8) . . ?
N5 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?

_refine_diff_density_max         2.215
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.174

_shelxl_version_number           2014/6


_chemical_name_systematic        
'(N,N,N-tris(2-pyridylmethyl)ethylenediamine-N-acetate)chromium(IV)peroxo diperhlorate'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: 33% H2O2 in water'
_chemical_properties_physical    
'rapid decomposition though loss of co-crystallised molecules and possible auto oxidation'
####################################################################### 
# 
# 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_publication_text
_database_code_depnum_ccdc_archive 'CCDC 1031522'
_audit_update_record             
;
2014-10-29 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_chemical_name_id                '[Cr(tpena)](ClO4)2(C4H8O2)0.5'
_chemical_name_common            1
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H24 Cr N5 O2, 0.5(C4 H8 O2), 2(Cl O4)'
_chemical_formula_sum            'C24 H28 Cl2 Cr N5 O11'
_chemical_formula_weight         685.41

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   16.3004(14)
_cell_length_b                   12.4635(11)
_cell_length_c                   13.5694(12)
_cell_angle_alpha                90
_cell_angle_beta                 91.647(5)
_cell_angle_gamma                90
_cell_volume                     2755.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9278

_cell_measurement_theta_min      2.53

_cell_measurement_theta_max      30.63


_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_F_000             1412
_exptl_transmission_factor_min   .
_exptl_transmission_factor_max   .
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.680
_shelx_estimated_absorpt_T_min   0.727
_shelx_estimated_absorpt_T_max   0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6980
_exptl_absorpt_correction_T_max  0.7461

_exptl_absorpt_process_details   'SADABS v2008/1 (Sheldrick, 2008)'

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed-tube'
_diffrn_measurement_device_type  'Bruker-Nonius X8APEX-II CCD'
_diffrn_measurement_method       'thin-slice ω and φ scans'
_diffrn_detector_area_resol_mean 9.1
_diffrn_reflns_number            88931
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.057
_diffrn_reflns_theta_max         30.706
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999

_reflns_number_total             8510
_reflns_number_gt                7533
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
Reflections were merged by SHELXL according to the crystal 
class for the calculation of statistics and refinement. 
 
_reflns_Friedel_fraction is defined as the number of unique 
Friedel pairs measured divided by the number that would be 
possible theoretically, ignoring centric projections and 
systematic absences. 
;

_computing_data_collection       'APEX2 v.2010.1-2 (Bruker Nonius, 2010)'
_computing_cell_refinement       'SAINT v.7.68a (Bruker, 2010)'
_computing_data_reduction        'SAINT v.7.68a (Bruker, 2010)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_molecular_graphics    
'Mercury 3.11 (Macrae at al., 2006) and POV-RAY (Cason, 2003)'
_computing_publication_material  'SHELX-2013 (Sheldrick, 2013)'

_refine_special_details          
; 
? 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0457P)²+1.5468P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8510
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0878
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.76198(2) 0.37981(2) 0.12953(2) 0.00800(5) Uani 1 1 d . . . . .
O1 O 0.93309(6) 0.35177(8) -0.07229(7) 0.01477(18) Uani 1 1 d . . . . .
N1 N 0.70117(6) 0.48465(9) 0.03568(7) 0.01132(19) Uani 1 1 d . . . . .
C1 C 0.63906(8) 0.46208(11) -0.02883(9) 0.0141(2) Uani 1 1 d . . . . .
H1 H 0.6213 0.3898 -0.0361 0.017 Uiso 1 1 calc R U . . .
Cl2 Cl 0.51361(2) 0.27595(2) 0.35586(2) 0.01392(7) Uani 1 1 d . . . . .
O2 O 0.82795(5) 0.32132(7) 0.02649(6) 0.01181(17) Uani 1 1 d . . . . .
N2 N 0.84537(6) 0.50426(8) 0.12749(7) 0.01022(18) Uani 1 1 d . . . . .
C2 C 0.60046(8) 0.54115(12) -0.08476(10) 0.0173(2) Uani 1 1 d . . . . .
H2 H 0.5564 0.5238 -0.1293 0.021 Uiso 1 1 calc R U . . .
Cl3 Cl 0.13601(2) 0.30746(2) 0.19107(2) 0.01577(7) Uani 1 1 d . . . . .
O3 O 0.07603(6) 0.55590(8) 0.50503(8) 0.0204(2) Uani 1 1 d . . . . .
N3 N 0.83694(6) 0.31539(8) 0.23822(7) 0.00984(18) Uani 1 1 d . . . . .
C3 C 0.62724(9) 0.64599(12) -0.07460(11) 0.0199(3) Uani 1 1 d . . . . .
H3 H 0.6013 0.7017 -0.1118 0.024 Uiso 1 1 calc R U . . .
O4 O 0.21792(6) 0.30565(9) 0.23431(9) 0.0250(2) Uani 1 1 d . . . . .
N4 N 0.70261(6) 0.44371(8) 0.24845(8) 0.01058(19) Uani 1 1 d . . . . .
C4 C 0.69226(8) 0.66931(11) -0.00971(10) 0.0174(2) Uani 1 1 d . . . . .
H4 H 0.7119 0.7408 -0.0029 0.021 Uiso 1 1 calc R U . . .
O5 O 0.13725(8) 0.26934(11) 0.09048(9) 0.0327(3) Uani 1 1 d . . . . .
N5 N 0.70800(6) 0.23029(8) 0.14344(8) 0.01067(19) Uani 1 1 d . . . . .
C5 C 0.72796(8) 0.58721(10) 0.04490(9) 0.0120(2) Uani 1 1 d . . . . .
O6 O 0.08223(6) 0.24127(9) 0.24765(9) 0.0244(2) Uani 1 1 d . . . . .
C6 C 0.79784(8) 0.60578(10) 0.11863(9) 0.0122(2) Uani 1 1 d . . . . .
H6A H 0.8335 0.6645 0.0958 0.015 Uiso 1 1 calc R U . . .
H6B H 0.7761 0.6261 0.1834 0.015 Uiso 1 1 calc R U . . .
O7 O 0.10561(7) 0.41658(8) 0.18997(8) 0.0221(2) Uani 1 1 d . . . . .
C7 C 0.89652(8) 0.49042(10) 0.03834(9) 0.0135(2) Uani 1 1 d . . . . .
H7A H 0.9549 0.5028 0.0571 0.016 Uiso 1 1 calc R U . . .
H7B H 0.8802 0.5451 -0.0114 0.016 Uiso 1 1 calc R U . . .
O8 O 0.49190(8) 0.31917(11) 0.26029(9) 0.0331(3) Uani 1 1 d . . . . .
C8 C 0.88765(7) 0.37999(10) -0.00715(9) 0.0116(2) Uani 1 1 d . . . . .
O9 O 0.47983(8) 0.34236(10) 0.43122(9) 0.0306(3) Uani 1 1 d . . . . .
C9 C 0.89784(7) 0.49379(10) 0.21997(9) 0.0124(2) Uani 1 1 d . . . . .
H9A H 0.8684 0.5224 0.2771 0.015 Uiso 1 1 calc R U . . .
H9B H 0.9495 0.5347 0.2135 0.015 Uiso 1 1 calc R U . . .
O10 O 0.60188(6) 0.27223(9) 0.36826(8) 0.0210(2) Uani 1 1 d . . . . .
C10 C 0.91643(7) 0.37554(10) 0.23487(9) 0.0127(2) Uani 1 1 d . . . . .
H10A H 0.9494 0.3485 0.1800 0.015 Uiso 1 1 calc R U . . .
H10B H 0.9484 0.3650 0.2973 0.015 Uiso 1 1 calc R U . . .
O11 O 0.48166(7) 0.16890(9) 0.36428(10) 0.0290(3) Uani 1 1 d . . . . .
C11 C 0.79810(8) 0.32778(10) 0.33649(9) 0.0118(2) Uani 1 1 d . . . . .
H11A H 0.7693 0.2605 0.3531 0.014 Uiso 1 1 calc R U . . .
H11B H 0.8414 0.3405 0.3878 0.014 Uiso 1 1 calc R U . . .
C12 C 0.73840(7) 0.41877(10) 0.33653(9) 0.0111(2) Uani 1 1 d . . . . .
C13 C 0.71716(8) 0.47003(11) 0.42315(9) 0.0144(2) Uani 1 1 d . . . . .
H13 H 0.7448 0.4533 0.4838 0.017 Uiso 1 1 calc R U . . .
C14 C 0.65496(8) 0.54599(11) 0.41954(10) 0.0166(2) Uani 1 1 d . . . . .
H14 H 0.6392 0.5820 0.4777 0.020 Uiso 1 1 calc R U . . .
C15 C 0.61593(8) 0.56868(11) 0.32931(10) 0.0161(2) Uani 1 1 d . . . . .
H15 H 0.5725 0.6195 0.3253 0.019 Uiso 1 1 calc R U . . .
C16 C 0.64113(7) 0.51641(10) 0.24588(10) 0.0137(2) Uani 1 1 d . . . . .
H16 H 0.6143 0.5321 0.1845 0.016 Uiso 1 1 calc R U . . .
C17 C 0.84484(7) 0.19943(10) 0.21368(9) 0.0121(2) Uani 1 1 d . . . . .
H17A H 0.8681 0.1595 0.2710 0.015 Uiso 1 1 calc R U . . .
H17B H 0.8817 0.1900 0.1576 0.015 Uiso 1 1 calc R U . . .
C18 C 0.76014(7) 0.15838(10) 0.18692(9) 0.0117(2) Uani 1 1 d . . . . .
C19 C 0.73670(8) 0.05329(11) 0.20462(10) 0.0158(2) Uani 1 1 d . . . . .
H19 H 0.7735 0.0047 0.2368 0.019 Uiso 1 1 calc R U . . .
C20 C 0.65840(9) 0.02036(11) 0.17449(10) 0.0176(3) Uani 1 1 d . . . . .
H20 H 0.6412 -0.0514 0.1852 0.021 Uiso 1 1 calc R U . . .
C21 C 0.60565(8) 0.09337(11) 0.12859(10) 0.0164(2) Uani 1 1 d . . . . .
H21 H 0.5523 0.0720 0.1064 0.020 Uiso 1 1 calc R U . . .
C22 C 0.63193(8) 0.19781(11) 0.11556(9) 0.0134(2) Uani 1 1 d . . . . .
H22 H 0.5952 0.2483 0.0860 0.016 Uiso 1 1 calc R U . . .
C23 C 0.07075(9) 0.44821(12) 0.46934(11) 0.0207(3) Uani 1 1 d . . . . .
H23A H 0.1227 0.4101 0.4853 0.025 Uiso 1 1 calc R U . . .
H23B H 0.0627 0.4489 0.3968 0.025 Uiso 1 1 calc R U . . .
C24 C -0.00037(9) 0.61041(11) 0.48477(12) 0.0214(3) Uani 1 1 d . . . . .
H24A H -0.0103 0.6152 0.4126 0.026 Uiso 1 1 calc R U . . .
H24B H 0.0029 0.6843 0.5113 0.026 Uiso 1 1 calc R U . . .


_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
Cr1 O2 1.9310(9) . ?
Cr1 N3 2.0516(10) . ?
Cr1 N1 2.0590(11) . ?
Cr1 N2 2.0631(10) . ?
Cr1 N4 2.0651(10) . ?
Cr1 N5 2.0717(11) . ?
O1 C8 1.2212(15) . ?
N1 C1 1.3489(15) . ?
N1 C5 1.3553(16) . ?
C1 C2 1.3841(18) . ?
C1 H1 0.9500 . ?
Cl2 O9 1.4376(11) . ?
Cl2 O11 1.4381(11) . ?
Cl2 O8 1.4390(11) . ?
Cl2 O10 1.4445(10) . ?
O2 C8 1.3098(15) . ?
N2 C6 1.4868(16) . ?
N2 C7 1.4988(15) . ?
N2 C9 1.5039(15) . ?
C2 C3 1.383(2) . ?
C2 H2 0.9500 . ?
Cl3 O6 1.4413(11) . ?
Cl3 O4 1.4430(11) . ?
Cl3 O5 1.4460(12) . ?
Cl3 O7 1.4474(11) . ?
O3 C23 1.4286(17) . ?
O3 C24 1.4381(18) . ?
N3 C17 1.4896(16) . ?
N3 C10 1.4988(16) . ?
N3 C11 1.5004(15) . ?
C3 C4 1.3891(19) . ?
C3 H3 0.9500 . ?
N4 C16 1.3508(16) . ?
N4 C12 1.3510(15) . ?
C4 C5 1.3820(18) . ?
C4 H4 0.9500 . ?
N5 C22 1.3482(16) . ?
N5 C18 1.3583(16) . ?
C5 C6 1.5121(17) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.5136(18) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 C10 1.5169(18) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.4943(17) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.3904(17) . ?
C13 C14 1.3870(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.3924(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.3791(18) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.5071(17) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.3872(18) . ?
C19 C20 1.3910(19) . ?
C19 H19 0.9500 . ?
C20 C21 1.387(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.3833(18) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.510(2) 3_566 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C23 1.510(2) 3_566 ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?

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
O2 Cr1 N3 92.31(4) . . ?
O2 Cr1 N1 93.43(4) . . ?
N3 Cr1 N1 163.57(4) . . ?
O2 Cr1 N2 83.88(4) . . ?
N3 Cr1 N2 85.69(4) . . ?
N1 Cr1 N2 79.64(4) . . ?
O2 Cr1 N4 174.03(4) . . ?
N3 Cr1 N4 82.64(4) . . ?
N1 Cr1 N4 90.60(4) . . ?
N2 Cr1 N4 92.54(4) . . ?
O2 Cr1 N5 88.46(4) . . ?
N3 Cr1 N5 80.11(4) . . ?
N1 Cr1 N5 115.40(4) . . ?
N2 Cr1 N5 163.58(4) . . ?
N4 Cr1 N5 93.78(4) . . ?
C1 N1 C5 119.36(11) . . ?
C1 N1 Cr1 127.45(9) . . ?
C5 N1 Cr1 113.17(8) . . ?
N1 C1 C2 121.89(12) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
O9 Cl2 O11 109.31(8) . . ?
O9 Cl2 O8 109.65(8) . . ?
O11 Cl2 O8 109.80(8) . . ?
O9 Cl2 O10 109.65(7) . . ?
O11 Cl2 O10 108.83(7) . . ?
O8 Cl2 O10 109.59(7) . . ?
C8 O2 Cr1 118.44(8) . . ?
C6 N2 C7 109.47(10) . . ?
C6 N2 C9 115.08(9) . . ?
C7 N2 C9 110.33(9) . . ?
C6 N2 Cr1 107.39(7) . . ?
C7 N2 Cr1 107.84(7) . . ?
C9 N2 Cr1 106.42(7) . . ?
C3 C2 C1 118.74(12) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
O6 Cl3 O4 110.13(7) . . ?
O6 Cl3 O5 109.88(7) . . ?
O4 Cl3 O5 109.93(8) . . ?
O6 Cl3 O7 109.27(7) . . ?
O4 Cl3 O7 109.35(7) . . ?
O5 Cl3 O7 108.24(7) . . ?
C23 O3 C24 109.61(10) . . ?
C17 N3 C10 113.46(9) . . ?
C17 N3 C11 109.87(9) . . ?
C10 N3 C11 111.28(9) . . ?
C17 N3 Cr1 105.81(7) . . ?
C10 N3 Cr1 106.26(7) . . ?
C11 N3 Cr1 109.92(7) . . ?
C2 C3 C4 119.58(12) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C16 N4 C12 118.58(11) . . ?
C16 N4 Cr1 127.05(9) . . ?
C12 N4 Cr1 113.73(8) . . ?
C5 C4 C3 119.13(13) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C22 N5 C18 118.86(11) . . ?
C22 N5 Cr1 129.36(9) . . ?
C18 N5 Cr1 111.78(8) . . ?
N1 C5 C4 121.28(12) . . ?
N1 C5 C6 116.10(11) . . ?
C4 C5 C6 122.61(11) . . ?
N2 C6 C5 107.71(10) . . ?
N2 C6 H6A 110.2 . . ?
C5 C6 H6A 110.2 . . ?
N2 C6 H6B 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
N2 C7 C8 112.64(10) . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N2 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
O1 C8 O2 124.31(12) . . ?
O1 C8 C7 120.28(11) . . ?
O2 C8 C7 115.39(10) . . ?
N2 C9 C10 107.58(10) . . ?
N2 C9 H9A 110.2 . . ?
C10 C9 H9A 110.2 . . ?
N2 C9 H9B 110.2 . . ?
C10 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
N3 C10 C9 108.69(10) . . ?
N3 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
N3 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.3 . . ?
C12 C11 N3 111.71(10) . . ?
C12 C11 H11A 109.3 . . ?
N3 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
N3 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
N4 C12 C13 122.04(12) . . ?
N4 C12 C11 116.03(10) . . ?
C13 C12 C11 121.80(11) . . ?
C14 C13 C12 118.90(12) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 119.00(12) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 119.11(12) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
N4 C16 C15 122.27(12) . . ?
N4 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
N3 C17 C18 107.38(10) . . ?
N3 C17 H17A 110.2 . . ?
C18 C17 H17A 110.2 . . ?
N3 C17 H17B 110.2 . . ?
C18 C17 H17B 110.2 . . ?
H17A C17 H17B 108.5 . . ?
N5 C18 C19 121.75(11) . . ?
N5 C18 C17 115.99(11) . . ?
C19 C18 C17 122.26(11) . . ?
C18 C19 C20 118.86(12) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.6 . . ?
C21 C20 C19 119.35(12) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C22 C21 C20 118.98(12) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
N5 C22 C21 122.17(12) . . ?
N5 C22 H22 118.9 . . ?
C21 C22 H22 118.9 . . ?
O3 C23 C24 110.73(12) . 3_566 ?
O3 C23 H23A 109.5 . . ?
C24 C23 H23A 109.5 3_566 . ?
O3 C23 H23B 109.5 . . ?
C24 C23 H23B 109.5 3_566 . ?
H23A C23 H23B 108.1 . . ?
O3 C24 C23 110.90(12) . 3_566 ?
O3 C24 H24A 109.5 . . ?
C23 C24 H24A 109.5 3_566 . ?
O3 C24 H24B 109.5 . . ?
C23 C24 H24B 109.5 3_566 . ?
H24A C24 H24B 108.0 . . ?

_refine_diff_density_max         0.616
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.103

_shelxl_version_number           2013-4


_chemical_name_systematic        
'N,N,N-tris(2-pyridylmethyl)ethylenediamine-N-acetate-chromium(III) diperchlorate'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
