# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1051121'
_audit_update_record             
;
2015-02-25 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H15 Cl3 Cr N5, C3 H7 N O'
_chemical_formula_sum            'C21 H22 Cl3 Cr N6 O'
_chemical_formula_weight         532.79

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   9.0372(2)
_cell_length_b                   12.0050(3)
_cell_length_c                   12.1284(3)
_cell_angle_alpha                87.5459(15)
_cell_angle_beta                 68.1978(12)
_cell_angle_gamma                71.7827(13)
_cell_volume                     1156.46(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3395
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      22.59

_exptl_crystal_description       block
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_F_000             546
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.868
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21213
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.792
_diffrn_reflns_theta_max         28.308
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5744
_reflns_number_gt                3635
_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       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_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)+(0.0597P)²+0.4956P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5744
_refine_ls_number_parameters     288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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 0.68007(6) 0.74506(4) 0.75697(4) 0.03475(15) Uani 1 1 d . . . . .
Cl2 Cl 0.44447(10) 0.80820(8) 0.92847(8) 0.0486(2) Uani 1 1 d . . . . .
Cl3 Cl 0.54002(11) 0.69555(9) 0.65131(8) 0.0516(2) Uani 1 1 d . . . . .
Cl4 Cl 0.65869(11) 0.93034(8) 0.69270(9) 0.0566(3) Uani 1 1 d . . . . .
N5 N 0.7363(3) 0.5800(2) 0.8088(2) 0.0326(5) Uani 1 1 d . . . . .
N6 N 0.8950(3) 0.5170(2) 0.7987(2) 0.0307(5) Uani 1 1 d . . . . .
C7 C 0.8995(4) 0.4085(3) 0.8371(3) 0.0370(7) Uani 1 1 d . . . . .
H7 H 0.9940 0.3490 0.8381 0.044 Uiso 1 1 calc R U . . .
C8 C 0.7394(4) 0.4028(3) 0.8743(3) 0.0425(8) Uani 1 1 d . . . . .
H8 H 0.7029 0.3400 0.9065 0.051 Uiso 1 1 calc R U . . .
C9 C 0.6431(4) 0.5108(3) 0.8536(3) 0.0393(7) Uani 1 1 d . . . . .
H9 H 0.5286 0.5317 0.8691 0.047 Uiso 1 1 calc R U . . .
N10 N 0.9108(3) 0.6747(2) 0.6147(2) 0.0369(6) Uani 1 1 d . . . . .
N11 N 1.0515(3) 0.6039(2) 0.6295(2) 0.0375(6) Uani 1 1 d . . . . .
C12 C 1.1932(4) 0.5948(3) 0.5318(3) 0.0484(9) Uani 1 1 d . . . . .
H12 H 1.3036 0.5552 0.5235 0.058 Uiso 1 1 calc R U . . .
C13 C 1.1376(6) 0.6586(4) 0.4443(3) 0.0671(10) Uani 1 1 d . . . . .
H13 H 1.2030 0.6671 0.3665 0.080 Uiso 1 1 calc R U . . .
C14 C 0.9555(5) 0.7073(3) 0.5044(3) 0.0494(9) Uani 1 1 d . . . . .
H14 H 0.8823 0.7539 0.4708 0.059 Uiso 1 1 calc R U . . .
N15 N 0.8322(3) 0.7617(2) 0.8472(2) 0.0339(6) Uani 1 1 d . . . . .
C16 C 0.9875(3) 0.6836(3) 0.8260(3) 0.0308(6) Uani 1 1 d . . . . .
C17 C 1.0975(4) 0.7174(3) 0.8599(3) 0.0446(8) Uani 1 1 d . . . . .
H17 H 1.2086 0.6696 0.8389 0.054 Uiso 1 1 calc R U . . .
C18 C 1.0405(6) 0.8220(4) 0.9247(4) 0.0692(12) Uani 1 1 d . . . . .
H18 H 1.1150 0.8452 0.9472 0.083 Uiso 1 1 calc R U . . .
C19 C 0.8845(6) 0.8918(4) 0.9570(5) 0.0789(14) Uani 1 1 d . . . . .
H19 H 0.8440 0.9591 1.0084 0.095 Uiso 1 1 calc R U . . .
C20 C 0.7887(5) 0.8618(3) 0.9130(3) 0.0533(9) Uani 1 1 d . . . . .
H20 H 0.6815 0.9146 0.9288 0.064 Uiso 1 1 calc R U . . .
C21 C 1.0340(3) 0.5691(3) 0.7525(3) 0.0309(6) Uani 1 1 d . . . . .
C22 C 1.1883(3) 0.4713(3) 0.7557(3) 0.0332(7) Uani 1 1 d . . . . .
C23 C 1.2175(4) 0.4557(3) 0.8610(3) 0.0395(7) Uani 1 1 d . . . . .
H23 H 1.1536 0.5121 0.9252 0.047 Uiso 1 1 calc R U . . .
C24 C 1.3406(4) 0.3574(3) 0.8715(3) 0.0485(9) Uani 1 1 d . . . . .
H24 H 1.3590 0.3484 0.9424 0.058 Uiso 1 1 calc R U . . .
C25 C 1.4357(5) 0.2731(3) 0.7776(4) 0.0565(10) Uani 1 1 d . . . . .
H25 H 1.5195 0.2078 0.7843 0.068 Uiso 1 1 calc R U . . .
C26 C 1.4064(4) 0.2858(3) 0.6742(4) 0.0544(10) Uani 1 1 d . . . . .
H26 H 1.4702 0.2286 0.6107 0.065 Uiso 1 1 calc R U . . .
C27 C 1.2819(4) 0.3836(3) 0.6633(3) 0.0442(8) Uani 1 1 d . . . . .
H27 H 1.2612 0.3902 0.5933 0.053 Uiso 1 1 calc R U . . .
O28 O 0.9525(6) 0.1516(4) 0.7972(5) 0.1444(19) Uani 1 1 d . . . . .
C29 C 0.9741(6) 0.0700(4) 0.7294(5) 0.0853(15) Uani 1 1 d . . . . .
H29 H 0.8804 0.0554 0.7266 0.102 Uiso 1 1 calc R U . . .
N30 N 1.1237(4) 0.0028(3) 0.6609(3) 0.0560(8) Uani 1 1 d . . . . .
C31 C 1.1429(6) -0.0962(4) 0.5857(5) 0.0841(14) Uani 1 1 d . . . . .
H31A H 1.2603 -0.1372 0.5436 0.126 Uiso 1 1 calc R U . . .
H31B H 1.0906 -0.0678 0.5296 0.126 Uiso 1 1 calc R U . . .
H31C H 1.0903 -0.1489 0.6344 0.126 Uiso 1 1 calc R U . . .
C32 C 1.2722(7) 0.0194(5) 0.6599(6) 0.108(2) Uani 1 1 d . . . . .
H32A H 1.3684 -0.0397 0.6056 0.162 Uiso 1 1 calc R U . . .
H32B H 1.2742 0.0133 0.7386 0.162 Uiso 1 1 calc R U . . .
H32C H 1.2749 0.0959 0.6349 0.162 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 N5 2.020(2) . ?
Cr1 N10 2.095(3) . ?
Cr1 N15 2.106(2) . ?
Cr1 Cl2 2.2958(9) . ?
Cr1 Cl4 2.2994(10) . ?
Cr1 Cl3 2.3103(10) . ?
N5 C9 1.325(4) . ?
N5 N6 1.357(3) . ?
N6 C7 1.359(4) . ?
N6 C21 1.490(4) . ?
C7 C8 1.370(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.389(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
N10 C14 1.326(4) . ?
N10 N11 1.361(3) . ?
N11 C12 1.361(4) . ?
N11 C21 1.496(4) . ?
C12 C13 1.432(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.458(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
N15 C20 1.337(4) . ?
N15 C16 1.358(4) . ?
C16 C17 1.376(4) . ?
C16 C21 1.525(4) . ?
C17 C18 1.356(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.313(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.311(6) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.529(4) . ?
C22 C27 1.386(4) . ?
C22 C23 1.390(4) . ?
C23 C24 1.385(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.374(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.368(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.390(5) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
O28 C29 1.226(6) . ?
C29 N30 1.308(6) . ?
C29 H29 0.9300 . ?
N30 C32 1.412(5) . ?
N30 C31 1.456(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

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
N5 Cr1 N10 83.11(10) . . ?
N5 Cr1 N15 81.74(10) . . ?
N10 Cr1 N15 83.65(10) . . ?
N5 Cr1 Cl2 91.20(7) . . ?
N10 Cr1 Cl2 172.46(8) . . ?
N15 Cr1 Cl2 90.66(7) . . ?
N5 Cr1 Cl4 171.08(7) . . ?
N10 Cr1 Cl4 90.63(8) . . ?
N15 Cr1 Cl4 91.29(7) . . ?
Cl2 Cr1 Cl4 94.46(4) . . ?
N5 Cr1 Cl3 90.34(7) . . ?
N10 Cr1 Cl3 90.82(8) . . ?
N15 Cr1 Cl3 170.81(7) . . ?
Cl2 Cr1 Cl3 94.16(4) . . ?
Cl4 Cr1 Cl3 96.12(4) . . ?
C9 N5 N6 106.4(2) . . ?
C9 N5 Cr1 131.9(2) . . ?
N6 N5 Cr1 121.74(18) . . ?
N5 N6 C7 110.0(2) . . ?
N5 N6 C21 121.0(2) . . ?
C7 N6 C21 129.0(2) . . ?
N6 C7 C8 107.4(3) . . ?
N6 C7 H7 126.3 . . ?
C8 C7 H7 126.3 . . ?
C7 C8 C9 105.4(3) . . ?
C7 C8 H8 127.3 . . ?
C9 C8 H8 127.3 . . ?
N5 C9 C8 110.8(3) . . ?
N5 C9 H9 124.6 . . ?
C8 C9 H9 124.6 . . ?
C14 N10 N11 108.2(3) . . ?
C14 N10 Cr1 127.5(2) . . ?
N11 N10 Cr1 122.93(19) . . ?
N10 N11 C12 111.9(3) . . ?
N10 N11 C21 117.3(2) . . ?
C12 N11 C21 129.4(3) . . ?
N11 C12 C13 106.0(3) . . ?
N11 C12 H12 127.0 . . ?
C13 C12 H12 127.0 . . ?
C12 C13 C14 104.5(3) . . ?
C12 C13 H13 127.7 . . ?
C14 C13 H13 127.7 . . ?
N10 C14 C13 109.1(3) . . ?
N10 C14 H14 125.4 . . ?
C13 C14 H14 125.4 . . ?
C20 N15 C16 117.3(3) . . ?
C20 N15 Cr1 119.2(2) . . ?
C16 N15 Cr1 122.51(19) . . ?
N15 C16 C17 118.6(3) . . ?
N15 C16 C21 116.6(2) . . ?
C17 C16 C21 124.4(3) . . ?
C18 C17 C16 118.6(3) . . ?
C18 C17 H17 120.7 . . ?
C16 C17 H17 120.7 . . ?
C19 C18 C17 122.6(4) . . ?
C19 C18 H18 118.7 . . ?
C17 C18 H18 118.7 . . ?
C20 C19 C18 116.6(4) . . ?
C20 C19 H19 121.7 . . ?
C18 C19 H19 121.7 . . ?
C19 C20 N15 125.5(4) . . ?
C19 C20 H20 117.3 . . ?
N15 C20 H20 117.3 . . ?
N6 C21 N11 108.6(2) . . ?
N6 C21 C16 110.2(2) . . ?
N11 C21 C16 105.1(2) . . ?
N6 C21 C22 104.4(2) . . ?
N11 C21 C22 113.2(2) . . ?
C16 C21 C22 115.4(2) . . ?
C27 C22 C23 118.0(3) . . ?
C27 C22 C21 120.9(3) . . ?
C23 C22 C21 119.9(3) . . ?
C24 C23 C22 120.9(3) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C25 C24 C23 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 119.7(3) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C27 120.5(3) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C22 C27 C26 120.6(3) . . ?
C22 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
O28 C29 N30 122.6(5) . . ?
O28 C29 H29 118.7 . . ?
N30 C29 H29 118.7 . . ?
C29 N30 C32 122.1(4) . . ?
C29 N30 C31 120.5(4) . . ?
C32 N30 C31 117.3(4) . . ?
N30 C31 H31A 109.5 . . ?
N30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N30 C32 H32A 109.5 . . ?
N30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_refine_diff_density_max         0.694
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.070

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1051122'
_audit_update_record             
;
2015-02-25 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H14 Cl3 Cr N6, 2(C3 H7 N O)'
_chemical_formula_sum            'C23 H28 Cl3 Cr N8 O2'
_chemical_formula_weight         606.88

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                   11.4170(13)
_cell_length_b                   14.1673(15)
_cell_length_c                   16.8852(19)
_cell_angle_alpha                90
_cell_angle_beta                 98.684(2)
_cell_angle_gamma                90
_cell_volume                     2699.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1380
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      19.25

_exptl_crystal_description       block
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             1252
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.758
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21459
_diffrn_reflns_av_unetI/netI     0.0931
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.804
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5019
_reflns_number_gt                3067
_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       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

_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)+(0.0907P)²+5.3017P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5019
_refine_ls_number_parameters     333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0712
_refine_ls_wR_factor_ref         0.2055
_refine_ls_wR_factor_gt          0.1725
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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 0.43062(8) 0.67264(6) 0.86859(5) 0.0221(3) Uani 1 1 d . . . . .
Cl2 Cl 0.53883(14) 0.68906(11) 0.99441(9) 0.0327(4) Uani 1 1 d . . . . .
Cl3 Cl 0.30178(14) 0.56400(11) 0.90779(9) 0.0323(4) Uani 1 1 d . . . . .
Cl4 Cl 0.30948(14) 0.80015(11) 0.88252(10) 0.0337(4) Uani 1 1 d . . . . .
N5 N 0.5388(4) 0.5670(3) 0.8414(3) 0.0222(11) Uani 1 1 d . . . . .
N6 N 0.5784(4) 0.5664(3) 0.7692(3) 0.0266(11) Uani 1 1 d . . . . .
C7 C 0.6405(6) 0.4873(4) 0.7566(4) 0.0302(14) Uani 1 1 d . . . . .
H7 H 0.6736 0.4733 0.7109 0.036 Uiso 1 1 calc R U . . .
C8 C 0.6456(7) 0.4294(5) 0.8267(5) 0.065(2) Uani 1 1 d . . . . .
H8 H 0.6821 0.3710 0.8369 0.078 Uiso 1 1 calc R U . . .
C9 C 0.5742(6) 0.4889(5) 0.8826(4) 0.0401(17) Uani 1 1 d . . . . .
H9 H 0.5598 0.4728 0.9337 0.048 Uiso 1 1 calc R U . . .
N10 N 0.3533(4) 0.6570(3) 0.7480(3) 0.0231(11) Uani 1 1 d . . . . .
C11 C 0.4189(5) 0.6543(4) 0.6867(3) 0.0216(11) Uani 1 1 d . . . . .
C12 C 0.3598(5) 0.6672(4) 0.6101(4) 0.0277(14) Uani 1 1 d . . . . .
H12 H 0.4009 0.6702 0.5666 0.033 Uiso 1 1 calc R U . . .
C13 C 0.2416(7) 0.6753(5) 0.5999(6) 0.058(2) Uani 1 1 d . . . . .
H13 H 0.2037 0.6843 0.5477 0.070 Uiso 1 1 calc R U . . .
C14 C 0.1782(10) 0.6722(6) 0.6525(6) 0.075(3) Uani 1 1 d . . . . .
H14 H 0.0959 0.6747 0.6420 0.090 Uiso 1 1 calc R U . . .
C15 C 0.2377(6) 0.6652(4) 0.7243(4) 0.0379(17) Uani 1 1 d . . . . .
H15 H 0.1920 0.6660 0.7654 0.046 Uiso 1 1 calc R U . . .
N16 N 0.5532(4) 0.7601(3) 0.8213(3) 0.0231(11) Uani 1 1 d . . . . .
C17 C 0.5884(5) 0.7422(4) 0.7496(3) 0.0212(10) Uani 1 1 d . . . . .
C18 C 0.6412(5) 0.8125(4) 0.7123(4) 0.0268(14) Uani 1 1 d . . . . .
H18 H 0.6572 0.8042 0.6604 0.032 Uiso 1 1 calc R U . . .
C19 C 0.6704(7) 0.8951(5) 0.7520(4) 0.0449(18) Uani 1 1 d . . . . .
H19 H 0.7079 0.9425 0.7271 0.054 Uiso 1 1 calc R U . . .
C20 C 0.6464(6) 0.9087(5) 0.8243(5) 0.0448(18) Uani 1 1 d . . . . .
H20 H 0.6725 0.9626 0.8532 0.054 Uiso 1 1 calc R U . . .
C21 C 0.5832(6) 0.8428(4) 0.8557(4) 0.0328(15) Uani 1 1 d . . . . .
H21 H 0.5587 0.8556 0.9047 0.039 Uiso 1 1 calc R U . . .
C22 C 0.5498(5) 0.6478(4) 0.7117(3) 0.0200(12) Uani 1 1 d . . . . .
N23 N 0.6127(4) 0.6264(3) 0.6439(3) 0.0268(11) Uani 1 1 d . . . . .
N24 N 0.5616(5) 0.5643(3) 0.5878(3) 0.0287(12) Uani 1 1 d . . . . .
C25 C 0.6438(6) 0.5364(5) 0.5466(4) 0.0369(16) Uani 1 1 d . . . . .
H25 H 0.6317 0.4953 0.5032 0.044 Uiso 1 1 calc R U . . .
C26 C 0.7600(7) 0.5805(6) 0.5795(5) 0.058(2) Uani 1 1 d . . . . .
H26 H 0.8328 0.5733 0.5619 0.069 Uiso 1 1 calc R U . . .
C27 C 0.7326(6) 0.6360(4) 0.6442(4) 0.0332(15) Uani 1 1 d . . . . .
H27 H 0.7851 0.6716 0.6797 0.040 Uiso 1 1 calc R U . . .
O28 O -0.0232(6) 0.6760(5) 0.4943(4) 0.081(2) Uani 1 1 d . . . . .
C29 C -0.0993(8) 0.7365(7) 0.4748(5) 0.065(2) Uani 1 1 d . . . . .
H29 H -0.1777 0.7202 0.4768 0.078 Uiso 1 1 calc R U . . .
N30 N -0.0776(5) 0.8245(4) 0.4507(4) 0.0480(16) Uani 1 1 d . . . . .
C31 C 0.0414(7) 0.8521(7) 0.4457(6) 0.069(3) Uani 1 1 d . . . . .
H31A H 0.0936 0.7998 0.4603 0.103 Uiso 1 1 calc R U . . .
H31B H 0.0635 0.9038 0.4816 0.103 Uiso 1 1 calc R U . . .
H31C H 0.0471 0.8713 0.3919 0.103 Uiso 1 1 calc R U . . .
C32 C -0.1717(8) 0.8890(7) 0.4273(6) 0.084(3) Uani 1 1 d . . . . .
H32A H -0.1752 0.9041 0.3716 0.126 Uiso 1 1 calc R U . . .
H32B H -0.1583 0.9456 0.4586 0.126 Uiso 1 1 calc R U . . .
H32C H -0.2453 0.8608 0.4360 0.126 Uiso 1 1 calc R U . . .
O33 O 0.9548(6) 0.7237(4) 0.7543(4) 0.0719(18) Uani 1 1 d . . . . .
C34 C 0.9812(8) 0.8029(7) 0.7804(5) 0.062(2) Uani 1 1 d . . . . .
H34 H 1.0026 0.8090 0.8356 0.074 Uiso 1 1 calc R U . . .
N35 N 0.9817(6) 0.8800(5) 0.7367(4) 0.0565(18) Uani 1 1 d . . . . .
C36 C 0.9516(10) 0.8768(8) 0.6505(5) 0.083(3) Uani 1 1 d . . . . .
H36A H 0.9333 0.8131 0.6338 0.125 Uiso 1 1 calc R U . . .
H36B H 1.0176 0.8989 0.6265 0.125 Uiso 1 1 calc R U . . .
H36C H 0.8841 0.9164 0.6340 0.125 Uiso 1 1 calc R U . . .
C37 C 1.0139(10) 0.9697(7) 0.7734(8) 0.106(4) Uani 1 1 d . . . . .
H37A H 1.0339 0.9617 0.8302 0.159 Uiso 1 1 calc R U . . .
H37B H 0.9484 1.0126 0.7621 0.159 Uiso 1 1 calc R U . . .
H37C H 1.0809 0.9948 0.7522 0.159 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 N5 2.036(5) . ?
Cr1 N10 2.106(5) . ?
Cr1 N16 2.115(5) . ?
Cr1 Cl3 2.2946(18) . ?
Cr1 Cl2 2.3026(17) . ?
Cr1 Cl4 2.3087(18) . ?
N5 C9 1.337(8) . ?
N5 N6 1.363(6) . ?
N6 C7 1.361(7) . ?
N6 C22 1.510(7) . ?
C7 C8 1.434(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.580(11) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
N10 C15 1.325(8) . ?
N10 C11 1.366(7) . ?
C11 C12 1.379(8) . ?
C11 C22 1.492(8) . ?
C12 C13 1.339(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.229(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.301(11) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
N16 C21 1.329(7) . ?
N16 C17 1.355(7) . ?
C17 C18 1.366(8) . ?
C17 C22 1.519(8) . ?
C18 C19 1.364(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.306(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.337(9) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 N23 1.472(7) . ?
N23 N24 1.358(7) . ?
N23 C27 1.375(8) . ?
N24 C25 1.311(8) . ?
C25 C26 1.496(11) . ?
C25 H25 0.9300 . ?
C26 C27 1.418(10) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
O28 C29 1.229(10) . ?
C29 N30 1.347(10) . ?
C29 H29 0.9300 . ?
N30 C32 1.419(10) . ?
N30 C31 1.429(9) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O33 C34 1.226(10) . ?
C34 N35 1.319(10) . ?
C34 H34 0.9300 . ?
N35 C37 1.437(11) . ?
N35 C36 1.445(11) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?

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
N5 Cr1 N10 83.38(18) . . ?
N5 Cr1 N16 83.50(18) . . ?
N10 Cr1 N16 84.29(18) . . ?
N5 Cr1 Cl3 90.53(14) . . ?
N10 Cr1 Cl3 90.88(14) . . ?
N16 Cr1 Cl3 172.71(14) . . ?
N5 Cr1 Cl2 91.32(14) . . ?
N10 Cr1 Cl2 172.44(14) . . ?
N16 Cr1 Cl2 89.77(13) . . ?
Cl3 Cr1 Cl2 94.56(6) . . ?
N5 Cr1 Cl4 172.33(14) . . ?
N10 Cr1 Cl4 90.61(13) . . ?
N16 Cr1 Cl4 91.19(13) . . ?
Cl3 Cr1 Cl4 94.33(7) . . ?
Cl2 Cr1 Cl4 94.20(7) . . ?
C9 N5 N6 110.2(5) . . ?
C9 N5 Cr1 129.6(4) . . ?
N6 N5 Cr1 120.0(3) . . ?
C7 N6 N5 113.3(5) . . ?
C7 N6 C22 126.6(5) . . ?
N5 N6 C22 120.1(4) . . ?
N6 C7 C8 107.4(6) . . ?
N6 C7 H7 126.3 . . ?
C8 C7 H7 126.3 . . ?
C7 C8 C9 103.2(6) . . ?
C7 C8 H8 128.4 . . ?
C9 C8 H8 128.4 . . ?
N5 C9 C8 105.9(6) . . ?
N5 C9 H9 127.1 . . ?
C8 C9 H9 127.1 . . ?
C15 N10 C11 114.2(5) . . ?
C15 N10 Cr1 122.4(4) . . ?
C11 N10 Cr1 122.5(4) . . ?
N10 C11 C12 117.4(5) . . ?
N10 C11 C22 115.3(5) . . ?
C12 C11 C22 127.0(5) . . ?
C13 C12 C11 118.3(7) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C14 C13 C12 126.6(10) . . ?
C14 C13 H13 116.7 . . ?
C12 C13 H13 116.7 . . ?
C13 C14 C15 113.2(10) . . ?
C13 C14 H14 123.4 . . ?
C15 C14 H14 123.4 . . ?
C14 C15 N10 130.1(8) . . ?
C14 C15 H15 114.9 . . ?
N10 C15 H15 114.9 . . ?
C21 N16 C17 117.7(5) . . ?
C21 N16 Cr1 119.5(4) . . ?
C17 N16 Cr1 122.0(4) . . ?
N16 C17 C18 119.1(5) . . ?
N16 C17 C22 115.7(5) . . ?
C18 C17 C22 124.7(5) . . ?
C19 C18 C17 119.4(6) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 121.0(7) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 118.0(7) . . ?
C19 C20 H20 121.0 . . ?
C21 C20 H20 121.0 . . ?
N16 C21 C20 124.1(6) . . ?
N16 C21 H21 118.0 . . ?
C20 C21 H21 118.0 . . ?
N23 C22 C11 112.2(4) . . ?
N23 C22 N6 105.0(4) . . ?
C11 C22 N6 109.8(4) . . ?
N23 C22 C17 111.4(4) . . ?
C11 C22 C17 106.2(4) . . ?
N6 C22 C17 112.4(4) . . ?
N24 N23 C27 112.9(5) . . ?
N24 N23 C22 117.9(5) . . ?
C27 N23 C22 125.4(5) . . ?
C25 N24 N23 107.4(5) . . ?
N24 C25 C26 110.0(6) . . ?
N24 C25 H25 125.0 . . ?
C26 C25 H25 125.0 . . ?
C27 C26 C25 103.4(6) . . ?
C27 C26 H26 128.3 . . ?
C25 C26 H26 128.3 . . ?
N23 C27 C26 106.1(6) . . ?
N23 C27 H27 126.9 . . ?
C26 C27 H27 126.9 . . ?
O28 C29 N30 124.9(8) . . ?
O28 C29 H29 117.6 . . ?
N30 C29 H29 117.6 . . ?
C29 N30 C32 120.9(7) . . ?
C29 N30 C31 119.4(7) . . ?
C32 N30 C31 119.7(7) . . ?
N30 C31 H31A 109.5 . . ?
N30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N30 C32 H32A 109.5 . . ?
N30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O33 C34 N35 125.3(8) . . ?
O33 C34 H34 117.4 . . ?
N35 C34 H34 117.4 . . ?
C34 N35 C37 121.0(8) . . ?
C34 N35 C36 121.1(8) . . ?
C37 N35 C36 117.9(8) . . ?
N35 C36 H36A 109.5 . . ?
N35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N35 C37 H37A 109.5 . . ?
N35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

_refine_diff_density_max         1.823
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.113

_shelxl_version_number           2013-4

