# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1482833'
_audit_update_record             
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
# local name eb15265
_audit_creation_date             2015-10-20
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H20 Cl2 Cr2 N4 O6'
_chemical_formula_sum            'C24 H20 Cl2 Cr2 N4 O6'
_chemical_formula_weight         635.34
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N2 O5 Cr2 Cl2 '
_chemical_oxdiff_usercomment     '@ 120 K 1960 (or 1950 as written on vial) '
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'
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'
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_H-M_alt        'P n n 2'
_space_group_name_Hall           'P 2 -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   7.81306(10)
_cell_length_b                   12.17220(15)
_cell_length_c                   13.10384(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1246.20(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    25916
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      32.7020
_cell_measurement_theta_min      4.2170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.3263
_exptl_crystal_size_mid          0.1812
_exptl_crystal_size_min          0.1783
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45650
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.892
_diffrn_reflns_theta_min         3.035
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -48.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248   24.0000 -166.7022 107

#__ type_ start__ end____ width___ exp.time_
  2 omega  -12.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   77.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
  3 omega  -12.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   77.0000   30.0000 105

#__ type_ start__ end____ width___ exp.time_
  4 omega  -20.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -99.0000    0.0000 79

#__ type_ start__ end____ width___ exp.time_
  5 omega    3.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311 -126.0000 -176.6475 72

#__ type_ start__ end____ width___ exp.time_
  6 omega   -4.00   92.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   38.0000  -30.0000 96

#__ type_ start__ end____ width___ exp.time_
  7 omega   17.00   94.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311 -154.0000  -85.2487 77

#__ type_ start__ end____ width___ exp.time_
  8 omega  -78.00  -29.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248  133.0000 -102.0130 49

#__ type_ start__ end____ width___ exp.time_
  9 omega  -91.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5248  -77.0000  150.0000 105

#__ type_ start__ end____ width___ exp.time_
 10 omega  -54.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -38.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
 11 omega  -54.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -38.0000   30.0000 95

#__ type_ start__ end____ width___ exp.time_
 12 omega  -20.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311  -99.0000   60.0000 79

#__ type_ start__ end____ width___ exp.time_
 13 omega   -8.00   31.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311 -113.0000   34.2842 39

#__ type_ start__ end____ width___ exp.time_
 14 omega   -8.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.9311   57.0000 -150.0000 97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0038168000
_diffrn_orient_matrix_UB_12      0.0432639000
_diffrn_orient_matrix_UB_13      0.0361701000
_diffrn_orient_matrix_UB_21      -0.0315923000
_diffrn_orient_matrix_UB_22      -0.0371701000
_diffrn_orient_matrix_UB_23      0.0372022000
_diffrn_orient_matrix_UB_31      0.0850270000
_diffrn_orient_matrix_UB_32      -0.0118985000
_diffrn_orient_matrix_UB_33      0.0154309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                4406
_reflns_number_total             4514
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 
;
 Flack x determined using 2032 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4514
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0215
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0275P)²+0.2734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0528
_refine_special_details          
;
H atoms were located in a difference map and freely refined.


 
#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
164_ALERT_4_G Nr. of Refined C-H H-Atoms in Heavy-Atom Struct.         10 Note
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  O1      ..        5.0 s.u.
795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence ..         C6 Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Th(Min) ...          1 Report
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         39 Note
#===============================================================================


;



_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.11448(3) 0.60190(2) 0.34453(2) 0.01116(6) Uani 1 1 d . . . . .
Cl1 Cl 0.07112(5) 0.79006(3) 0.35851(3) 0.01674(8) Uani 1 1 d . . . . .
O1 O 0.13067(13) 0.43969(9) 0.34767(11) 0.01313(19) Uani 1 1 d . . . . .
O2 O 0.35903(16) 0.61555(10) 0.31449(10) 0.0164(2) Uani 1 1 d . . . . .
O3 O 0.55060(18) 0.62782(13) 0.18776(12) 0.0247(3) Uani 1 1 d . . . . .
N1 N 0.17236(19) 0.57707(12) 0.49764(11) 0.0138(3) Uani 1 1 d . . . . .
N2 N 0.10010(18) 0.61722(12) 0.18915(11) 0.0131(3) Uani 1 1 d . . . . .
C1 C 0.1598(2) 0.64975(15) 0.57515(13) 0.0169(3) Uani 1 1 d . . . . .
H1 H 0.114(3) 0.717(2) 0.558(2) 0.018(6) Uiso 1 1 d . . . . .
C2 C 0.2108(3) 0.62383(17) 0.67349(14) 0.0215(4) Uani 1 1 d . . . . .
H2 H 0.206(3) 0.681(2) 0.731(2) 0.025(6) Uiso 1 1 d . . . . .
C3 C 0.2776(3) 0.51999(16) 0.69276(14) 0.0228(4) Uani 1 1 d . . . . .
H3 H 0.318(4) 0.509(2) 0.757(2) 0.036(7) Uiso 1 1 d . . . . .
C4 C 0.2900(2) 0.44495(16) 0.61328(15) 0.0199(3) Uani 1 1 d . . . . .
H4 H 0.334(3) 0.377(2) 0.626(2) 0.018(6) Uiso 1 1 d . . . . .
C5 C 0.2368(2) 0.47586(14) 0.51607(13) 0.0145(3) Uani 1 1 d . . . . .
C6 C 0.2470(2) 0.40198(14) 0.42422(14) 0.0155(3) Uani 1 1 d . . . . .
H6A H 0.359(3) 0.3990(17) 0.3954(19) 0.010(5) Uiso 1 1 d . . . . .
H6B H 0.211(3) 0.320(2) 0.4446(19) 0.017(5) Uiso 1 1 d . . . . .
C7 C -0.0415(2) 0.62843(14) 0.13166(13) 0.0156(3) Uani 1 1 d . . . . .
H7 H -0.152(3) 0.629(2) 0.170(2) 0.016(6) Uiso 1 1 d . . . . .
C8 C -0.0300(3) 0.63733(15) 0.02576(14) 0.0198(3) Uani 1 1 d . . . . .
H8 H -0.127(3) 0.644(2) -0.013(2) 0.026(7) Uiso 1 1 d . . . . .
C9 C 0.1296(3) 0.63084(17) -0.01997(14) 0.0224(4) Uani 1 1 d . . . . .
H9 H 0.139(3) 0.634(2) -0.091(2) 0.023(6) Uiso 1 1 d . . . . .
C10 C 0.2753(3) 0.62073(16) 0.03981(15) 0.0205(3) Uani 1 1 d . . . . .
H10 H 0.387(4) 0.619(2) 0.014(3) 0.032(8) Uiso 1 1 d . . . . .
C11 C 0.2558(2) 0.61689(14) 0.14491(13) 0.0154(3) Uani 1 1 d . . . . .
C12 C 0.4041(2) 0.61932(15) 0.21910(15) 0.0168(3) Uani 1 1 d . . . . .


_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 Cl1 2.3224(4) . ?
Cr1 O1 1.9789(11) . ?
Cr1 O1 1.9816(10) 2_565 ?
Cr1 O2 1.9579(13) . ?
Cr1 N1 2.0788(15) . ?
Cr1 N2 2.0477(15) . ?
O1 Cr1 1.9816(10) 2_565 ?
O1 C6 1.429(2) . ?
O2 C12 1.300(2) . ?
O3 C12 1.220(2) . ?
N1 C1 1.351(2) . ?
N1 C5 1.352(2) . ?
N2 C7 1.345(2) . ?
N2 C11 1.348(2) . ?
C1 H1 0.92(3) . ?
C1 C2 1.385(2) . ?
C2 H2 1.02(3) . ?
C2 C3 1.391(3) . ?
C3 H3 0.91(3) . ?
C3 C4 1.389(3) . ?
C4 H4 0.92(3) . ?
C4 C5 1.392(2) . ?
C5 C6 1.505(2) . ?
C6 H6A 0.95(3) . ?
C6 H6B 1.07(2) . ?
C7 H7 1.00(2) . ?
C7 C8 1.395(2) . ?
C8 H8 0.92(3) . ?
C8 C9 1.386(3) . ?
C9 H9 0.94(3) . ?
C9 C10 1.387(3) . ?
C10 H10 0.94(3) . ?
C10 C11 1.386(2) . ?
C11 C12 1.513(3) . ?

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
O1 Cr1 Cl1 172.57(4) . . ?
O1 Cr1 Cl1 96.28(3) 2_565 . ?
O1 Cr1 O1 78.84(5) . 2_565 ?
O1 Cr1 N1 79.68(6) . . ?
O1 Cr1 N1 98.80(6) 2_565 . ?
O1 Cr1 N2 89.48(6) 2_565 . ?
O1 Cr1 N2 96.61(6) . . ?
O2 Cr1 Cl1 94.28(4) . . ?
O2 Cr1 O1 165.73(6) . 2_565 ?
O2 Cr1 O1 91.51(5) . . ?
O2 Cr1 N1 89.66(6) . . ?
O2 Cr1 N2 81.14(6) . . ?
N1 Cr1 Cl1 95.68(4) . . ?
N2 Cr1 Cl1 88.89(4) . . ?
N2 Cr1 N1 170.02(6) . . ?
Cr1 O1 Cr1 101.11(5) . 2_565 ?
C6 O1 Cr1 123.17(11) . 2_565 ?
C6 O1 Cr1 112.07(10) . . ?
C12 O2 Cr1 117.45(11) . . ?
C1 N1 Cr1 127.94(12) . . ?
C1 N1 C5 119.30(15) . . ?
C5 N1 Cr1 112.69(11) . . ?
C7 N2 Cr1 127.67(12) . . ?
C7 N2 C11 120.12(16) . . ?
C11 N2 Cr1 112.20(11) . . ?
N1 C1 H1 114.8(17) . . ?
N1 C1 C2 121.97(17) . . ?
C2 C1 H1 123.2(17) . . ?
C1 C2 H2 121.3(15) . . ?
C1 C2 C3 118.94(18) . . ?
C3 C2 H2 119.7(15) . . ?
C2 C3 H3 116.0(19) . . ?
C4 C3 C2 119.20(17) . . ?
C4 C3 H3 124.7(19) . . ?
C3 C4 H4 118.8(17) . . ?
C3 C4 C5 119.19(17) . . ?
C5 C4 H4 122.0(17) . . ?
N1 C5 C4 121.39(16) . . ?
N1 C5 C6 114.92(15) . . ?
C4 C5 C6 123.69(16) . . ?
O1 C6 C5 109.62(13) . . ?
O1 C6 H6A 108.5(15) . . ?
O1 C6 H6B 107.8(13) . . ?
C5 C6 H6A 112.8(14) . . ?
C5 C6 H6B 110.0(13) . . ?
H6A C6 H6B 107.9(18) . . ?
N2 C7 H7 115.2(15) . . ?
N2 C7 C8 120.82(17) . . ?
C8 C7 H7 124.0(15) . . ?
C7 C8 H8 120.7(18) . . ?
C9 C8 C7 118.92(17) . . ?
C9 C8 H8 120.3(18) . . ?
C8 C9 H9 119.8(17) . . ?
C8 C9 C10 119.94(17) . . ?
C10 C9 H9 120.3(17) . . ?
C9 C10 H10 124(2) . . ?
C11 C10 C9 118.30(18) . . ?
C11 C10 H10 118(2) . . ?
N2 C11 C10 121.75(17) . . ?
N2 C11 C12 114.53(15) . . ?
C10 C11 C12 123.62(17) . . ?
O2 C12 C11 114.18(15) . . ?
O3 C12 O2 125.52(18) . . ?
O3 C12 C11 120.25(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C6 C5 -85.23(15) 2_565 . . . ?
Cr1 O1 C6 C5 35.66(16) . . . . ?
Cr1 O2 C12 O3 179.90(15) . . . . ?
Cr1 O2 C12 C11 2.3(2) . . . . ?
Cr1 N1 C1 C2 -176.81(14) . . . . ?
Cr1 N1 C5 C4 177.34(14) . . . . ?
Cr1 N1 C5 C6 -2.12(18) . . . . ?
Cr1 N2 C7 C8 -179.61(13) . . . . ?
Cr1 N2 C11 C10 176.66(14) . . . . ?
Cr1 N2 C11 C12 -7.02(19) . . . . ?
N1 C1 C2 C3 0.3(3) . . . . ?
N1 C5 C6 O1 -21.3(2) . . . . ?
N2 C7 C8 C9 2.1(3) . . . . ?
N2 C11 C12 O2 3.4(2) . . . . ?
N2 C11 C12 O3 -174.32(17) . . . . ?
C1 N1 C5 C4 0.2(2) . . . . ?
C1 N1 C5 C6 -179.31(16) . . . . ?
C1 C2 C3 C4 -0.5(3) . . . . ?
C2 C3 C4 C5 0.6(3) . . . . ?
C3 C4 C5 N1 -0.4(3) . . . . ?
C3 C4 C5 C6 179.01(17) . . . . ?
C4 C5 C6 O1 159.25(16) . . . . ?
C5 N1 C1 C2 -0.1(3) . . . . ?
C7 N2 C11 C10 -4.3(3) . . . . ?
C7 N2 C11 C12 172.06(15) . . . . ?
C7 C8 C9 C10 -2.9(3) . . . . ?
C8 C9 C10 C11 0.3(3) . . . . ?
C9 C10 C11 N2 3.3(3) . . . . ?
C9 C10 C11 C12 -172.63(17) . . . . ?
C10 C11 C12 O2 179.66(17) . . . . ?
C10 C11 C12 O3 1.9(3) . . . . ?
C11 N2 C7 C8 1.5(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
10 6 -3 0.1291 10.2831 5.6955 -2.5136 0.1162 -0.6301 0.7678
0 -14 11 0.0886 -0.1414 -13.5234 11.3648 -0.1735 0.9299 0.3243
-10 4 -6 0.1084 -10.0359 4.4103 -5.9477 0.0140 -0.0681 -0.9976
1 14 -11 0.0867 0.9224 13.5550 -11.2179 0.1772 -0.9503 -0.2560
4 -11 -13 0.1034 3.6448 -11.0620 -12.7342 -0.9531 -0.1777 0.2450
-3 -8 -15 0.1042 -3.2602 -8.1206 -15.3355 -0.8936 -0.1657 -0.4172
-10 5 -3 0.1222 -10.3832 4.8118 -3.3348 0.1272 0.0251 -0.9916
-1 10 15 0.0705 -0.8178 10.4139 14.6241 0.9826 0.1828 0.0322
9 -9 -5 0.1446 8.9937 -8.9892 -4.9890 -0.6037 -0.1356 0.7947
9 1 11 0.1840 8.9880 1.0041 11.0000 0.4070 0.0879 0.9220
9 3 -11 0.1169 8.9934 3.0019 -10.9862 -0.3018 -0.8044 0.5594
10 1 -6 0.1285 9.9914 1.0040 -5.9884 -0.2113 -0.5758 0.7452
-1 7 -17 0.1042 -0.9957 6.9938 -16.9906 -0.3082 -0.8606 -0.4301
-3 -15 -8 0.1093 -2.9926 -14.9909 -7.9961 -0.9264 0.3543 -0.1995
-9 -7 -7 0.1187 -8.9881 -6.9996 -7.0020 -0.5218 0.2836 -0.7890
2 -6 -17 0.0918 2.0034 -5.9953 -16.9872 -0.8815 -0.4724 -0.0205

_olex2_date_sample_submission    2015-10-09
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id '1960 (1950 on vial)'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1540438'
_audit_update_record             
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
# local name eb16140
_audit_creation_date             2016-05-02
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C11 H11 Cl2 Cr N2 O), 2(C5 H5 N)'
_chemical_formula_sum            'C32 H32 Cl4 Cr2 N6 O2'
_chemical_formula_weight         778.43
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl'
_chemical_oxdiff_usercomment     '@ 120 K 589'
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'
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'
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_H-M_alt        'I 41'
_space_group_name_Hall           'I 4bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'

_cell_length_a                   16.2418(2)
_cell_length_b                   16.2418(2)
_cell_length_c                   25.6069(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6755.0(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7432
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      74.7900
_cell_measurement_theta_min      5.1490
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.539
_exptl_absorpt_correction_T_max  0.7789
_exptl_absorpt_correction_T_min  0.3885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1121 before and 0.0825 after correction.
The Ratio of minimum to maximum transmission is 0.4988.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-9 -2 -9 0.0939
0 -7 12 0.0905
7 -1 12 0.0877
2 8 -11 0.0264
-5 7 10 0.0361
5 -7 -10 0.0098

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of pyridine and diethyl ether by vapour diffusion'
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.046
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-9.0000 -2.0001 -9.0012 -0.0275 0.1759 1.0138
0.0000 -7.0000 11.9994 0.1781 -0.9601 -0.0904
7.0000 -0.9999 12.0007 0.1124 -0.5091 -0.8370
2.0000 8.0000 -10.9990 -0.1881 0.9989 -0.1266
-5.0000 6.9999 9.9996 0.9928 0.1953 -0.0534
5.0000 -6.9999 -9.9996 -0.9928 -0.1953 0.0534

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            28737
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.316
_diffrn_reflns_theta_min         3.222
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -122.00  -6.00   1.00    5.00    --  -43.17 -19.00 150.00  116
  2  ω   -113.00 -17.00   1.00    5.00    --  -43.17 -57.00 -60.00   96
  3  ω    -70.00  27.00   1.00    5.00    --  -43.17  57.00  90.00   97
  4  ω     87.00 178.00   1.00   20.00    --  111.00  45.00-120.00   91
  5  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00-120.00  105
  6  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00   0.00  105
  7  ω     30.00 109.00   1.00   20.00    --  111.00 -94.00-150.00   79
  8  ω     36.00 135.00   1.00   20.00    --  111.00 -30.00  30.00   99
  9  ω     87.00 178.00   1.00   20.00    --  111.00  45.00   0.00   91
 10  ω     40.00 135.00   1.00   20.00    --  111.00 -45.00 -90.00   95
 11  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00 120.00  105
 12  ω     94.00 178.00   1.00   20.00    --  111.00 125.00 -60.00   84
 13  ω     30.00 109.00   1.00   20.00    --  111.00 -94.00 -30.00   79
 14  ω    106.00 160.00   1.00   20.00    --  111.00 125.00-180.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0493161000
_diffrn_orient_matrix_UB_12      0.0465783000
_diffrn_orient_matrix_UB_13      0.0420147000
_diffrn_orient_matrix_UB_21      -0.0015276000
_diffrn_orient_matrix_UB_22      0.0769691000
_diffrn_orient_matrix_UB_23      -0.0351145000
_diffrn_orient_matrix_UB_31      -0.0810507000
_diffrn_orient_matrix_UB_32      -0.0298702000
_diffrn_orient_matrix_UB_33      -0.0249563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5590
_reflns_number_total             6396
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6396
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0739
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1092P)²+21.3008P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1952
_refine_ls_wR_factor_ref         0.2107
_refine_special_details          
;
The model was refined as a merohedral, racemic twin.

The pyridine solvent molecules were modelled using an idealized hexagonal constraint.  All N and C atoms were refined with appropriate displacement ellipsoid (RIGU) restraints.  

The chloride ligands were modelled over two sites as indicated by peaks in a difference map.  There is a hing at further disorder corresponding to an interchange of pyridine with hmp ligands but this could not be modelled successfully.

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............    0.02427 Ang.

Probably an effect of multiple twinning.

#===============================================================================
034_ALERT_1_C No Flack Parameter Given. Z > Si, NonCentro ....     Please Do !

Consequence of the way the twinning was handled, see above.

090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       8.36 Note

Probably an effect of multiple twinning.


241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        C17 Check
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        C19 Check
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        C22 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....         N3 Check
242_ALERT_2_C Low       Ueq as Compared to Neighbors for .....         N4 Check
243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors of         C25 Check
243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors of         C30 Check
244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of          N5 Check
244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors of         C24 Check
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.0 Note
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.1 Note

Use of displacement ellipsoid restraints discussed above.

#===============================================================================
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         40 Report


Use of displacement ellipsoid restraints discussed above.


042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.11 Report
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      21.30 Why ?
111_ALERT_2_G ADDSYM Detects New (Pseudo) Centre of Symmetry .         90 %Fit

There is no higher symmetry; solutions in higher symmetry space groups have
fundamental chemical problems caused by the extra symmetry.

232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  Cl1     ..        6.7 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  Cl2     ..        7.3 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr2    --  Cl3     ..        6.7 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr2    --  Cl4A    ..       13.2 s.u.


Use of displacement ellipsoid restraints discussed above.


301_ALERT_3_G Main Residue  Disorder ............ Percentage =         12 Note
432_ALERT_2_G Short Inter X...Y Contact  Cl1A   ..  C32     ..       2.92 Ang.
432_ALERT_2_G Short Inter X...Y Contact  Cl4A   ..  C27     ..       3.23 Ang.

Disorder discussed above

432_ALERT_2_G Short Inter X...Y Contact  C17    ..  C23     ..       3.19 Ang.
802_ALERT_4_G CIF Input Record(s) with more than 80 Characters          2 Info
860_ALERT_3_G Number of Least-Squares Restraints .............        247 Note
870_ALERT_4_G ALERTS Related to Twinning Effects Suppressed ..          ! Info
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         20 Note
931_ALERT_5_G Found Twin Law ( 0 1  0)[       ] Estimated BASF       0.49 Check

Twinning discussed above.

#===============================================================================
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.41(3) 0.097(19) 0.089(19) 0.400(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Rigid body (RIGU) restrains
 N5, C23, C24, C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C28, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C18, C19, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, N3, C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, N1, C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl3A)=Sof(Cl4A)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl4)=FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C17(H17A,H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30), C31(H31), C32(H32)
5.c Fitted hexagon refined as free rotating group:
 N5(C23,C24,C25,C26,C27), N6(C28,C29,C30,C31,C32)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.05851(17) 0.42623(16) 0.62528(9) 0.0404(6) Uani 1 1 d . . . . .
Cl1A Cl 0.2176(12) 0.4701(17) 0.6420(9) 0.076(7) Uani 0.283(13) 1 d . . P A 2
Cl2A Cl 0.0862(19) 0.3008(13) 0.6212(8) 0.073(7) Uani 0.283(13) 1 d . . P A 2
O1 O 0.0617(7) 0.5476(6) 0.6220(4) 0.041(2) Uani 1 1 d . U . . .
N1 N 0.0772(8) 0.4408(7) 0.5464(5) 0.041(3) Uani 1 1 d . U . . .
N2 N 0.0483(7) 0.4155(7) 0.7062(5) 0.039(2) Uani 1 1 d . U . . .
C1 C 0.0683(11) 0.3841(10) 0.5056(6) 0.051(3) Uani 1 1 d . U . . .
H1 H 0.0410 0.3333 0.5118 0.061 Uiso 1 1 calc R . . . .
C2 C 0.0992(11) 0.4015(11) 0.4556(6) 0.056(3) Uani 1 1 d . U . . .
H2 H 0.0953 0.3628 0.4279 0.067 Uiso 1 1 calc R . . . .
C3 C 0.1371(11) 0.4805(11) 0.4481(7) 0.060(4) Uani 1 1 d . U . . .
H3 H 0.1589 0.4945 0.4148 0.072 Uiso 1 1 calc R . . . .
C4 C 0.1422(10) 0.5331(11) 0.4862(7) 0.053(3) Uani 1 1 d . U . . .
H4 H 0.1668 0.5853 0.4800 0.064 Uiso 1 1 calc R . . . .
C5 C 0.1128(9) 0.5150(8) 0.5353(5) 0.037(3) Uani 1 1 d . U . . .
C6 C 0.1124(7) 0.5753(6) 0.5810(4) 0.033(2) Uani 1 1 d . U . . .
H6A H 0.1693 0.5823 0.5941 0.039 Uiso 1 1 calc R . . . .
H6B H 0.0925 0.6296 0.5688 0.039 Uiso 1 1 calc R . . . .
C7 C 0.0996(11) 0.4526(11) 0.7358(6) 0.060(4) Uani 1 1 d . U . . .
H7 H 0.1398 0.4874 0.7203 0.072 Uiso 1 1 calc R . . . .
C8 C 0.0988(11) 0.4444(10) 0.7873(7) 0.059(4) Uani 1 1 d . U . . .
H8 H 0.1343 0.4776 0.8080 0.071 Uiso 1 1 calc R . . . .
C9 C 0.0464(13) 0.3875(12) 0.8115(8) 0.065(4) Uani 1 1 d . U . . .
H9 H 0.0501 0.3775 0.8480 0.078 Uiso 1 1 calc R . . . .
C10 C -0.0089(11) 0.3476(11) 0.7821(6) 0.053(4) Uani 1 1 d . U . . .
H10 H -0.0467 0.3092 0.7965 0.064 Uiso 1 1 calc R . . . .
C11 C -0.0077(8) 0.3662(10) 0.7281(6) 0.042(3) Uani 1 1 d . U . . .
H11 H -0.0487 0.3425 0.7063 0.051 Uiso 1 1 calc R . . . .
Cr2 Cr 0.43479(19) 0.56692(19) 0.37792(9) 0.0560(10) Uani 1 1 d . . . . .
Cl3A Cl 0.3021(5) 0.5891(5) 0.3736(3) 0.037(2) Uani 0.470(14) 1 d . . P B 2
Cl4A Cl 0.4653(6) 0.7147(4) 0.3906(3) 0.038(2) Uani 0.470(14) 1 d . . P B 2
O2 O 0.5558(7) 0.5538(8) 0.3769(5) 0.058(3) Uani 1 1 d . U . . .
N3 N 0.4510(8) 0.5815(8) 0.2983(5) 0.043(3) Uani 1 1 d . U . . .
N4 N 0.4181(8) 0.5503(9) 0.4580(5) 0.045(3) Uani 1 1 d . U . . .
C12 C 0.3961(12) 0.5537(12) 0.2632(6) 0.065(4) Uani 1 1 d . U . . .
H12 H 0.3528 0.5196 0.2755 0.078 Uiso 1 1 calc R . . . .
C13 C 0.3983(12) 0.5711(14) 0.2111(6) 0.074(5) Uani 1 1 d . U . . .
H13 H 0.3570 0.5519 0.1878 0.089 Uiso 1 1 calc R . . . .
C14 C 0.4629(11) 0.6176(11) 0.1941(7) 0.058(4) Uani 1 1 d . U . . .
H14 H 0.4683 0.6311 0.1582 0.070 Uiso 1 1 calc R . . . .
C15 C 0.5210(13) 0.6451(13) 0.2302(7) 0.066(5) Uani 1 1 d . U . . .
H15 H 0.5646 0.6806 0.2200 0.079 Uiso 1 1 calc R . . . .
C16 C 0.5133(13) 0.6193(15) 0.2802(8) 0.071(5) Uani 1 1 d . U . . .
C17 C 0.5739(12) 0.6149(14) 0.3299(8) 0.082(5) Uani 1 1 d . U . . .
H17A H 0.6295 0.6016 0.3166 0.099 Uiso 1 1 calc R . . . .
H17B H 0.5769 0.6711 0.3448 0.099 Uiso 1 1 calc R . . . .
C18 C 0.4431(13) 0.6039(12) 0.4912(6) 0.072(5) Uani 1 1 d . U . . .
H18 H 0.4765 0.6486 0.4799 0.086 Uiso 1 1 calc R . . . .
C19 C 0.4213(18) 0.5969(14) 0.5448(7) 0.093(7) Uani 1 1 d . U . . .
H19 H 0.4405 0.6364 0.5693 0.111 Uiso 1 1 calc R . . . .
C20 C 0.3753(13) 0.5371(12) 0.5599(7) 0.069(4) Uani 1 1 d . U . . .
H20 H 0.3556 0.5350 0.5948 0.083 Uiso 1 1 calc R . . . .
C21 C 0.3549(14) 0.4755(14) 0.5246(8) 0.072(5) Uani 1 1 d . U . . .
H21 H 0.3296 0.4259 0.5359 0.086 Uiso 1 1 calc R . . . .
C22 C 0.3719(17) 0.4880(14) 0.4738(8) 0.077(6) Uani 1 1 d . U . . .
H22 H 0.3502 0.4510 0.4486 0.092 Uiso 1 1 calc R . . . .
Cl1 Cl 0.2003(3) 0.4137(3) 0.63304(19) 0.0332(13) Uani 0.717(13) 1 d . . P A 1
Cl2 Cl 0.0351(4) 0.2850(3) 0.6153(2) 0.0353(13) Uani 0.717(13) 1 d . . P A 1
Cl3 Cl 0.2867(5) 0.5403(9) 0.3655(4) 0.058(3) Uani 0.530(14) 1 d . . P B 1
Cl4 Cl 0.4143(7) 0.7012(5) 0.3812(5) 0.058(3) Uani 0.530(14) 1 d . . P B 1
N5 N 0.6043(8) 0.7453(10) 0.5052(6) 0.101(8) Uani 1 1 d . U . . .
C23 C 0.6601(12) 0.7422(10) 0.5463(5) 0.134(9) Uani 1 1 d G U . . .
H23 H 0.6409 0.7362 0.5811 0.160 Uiso 1 1 calc R . . . .
C24 C 0.7441(11) 0.7478(12) 0.5364(7) 0.134(9) Uani 1 1 d G U . . .
H24 H 0.7822 0.7457 0.5645 0.160 Uiso 1 1 calc R . . . .
C25 C 0.7722(8) 0.7566(14) 0.4854(9) 0.196(16) Uani 1 1 d G U . . .
H25 H 0.8296 0.7605 0.4787 0.235 Uiso 1 1 calc R . . . .
C26 C 0.7164(11) 0.7598(12) 0.4444(6) 0.149(10) Uani 1 1 d G U . . .
H26 H 0.7356 0.7658 0.4095 0.178 Uiso 1 1 calc R . . . .
C27 C 0.6324(10) 0.7541(10) 0.4542(5) 0.122(8) Uani 1 1 d G U . . .
H27 H 0.5942 0.7563 0.4261 0.146 Uiso 1 1 calc R . . . .
N6 N 0.1032(4) 0.7636(7) 0.5030(3) 0.053(3) Uani 1 1 d . U . . .
C28 C 0.1671(6) 0.7747(7) 0.5384(3) 0.055(3) Uani 1 1 d G U . . .
H28 H 0.1552 0.7841 0.5743 0.066 Uiso 1 1 calc R . . . .
C29 C 0.2483(5) 0.7721(9) 0.5214(4) 0.073(5) Uani 1 1 d G U . . .
H29 H 0.2920 0.7797 0.5456 0.087 Uiso 1 1 calc R . . . .
C30 C 0.2656(4) 0.7584(10) 0.4690(5) 0.103(8) Uani 1 1 d G U . . .
H30 H 0.3212 0.7566 0.4573 0.123 Uiso 1 1 calc R . . . .
C31 C 0.2018(6) 0.7473(8) 0.4336(3) 0.071(5) Uani 1 1 d G U . . .
H31 H 0.2136 0.7379 0.3977 0.086 Uiso 1 1 calc R . . . .
C32 C 0.1205(5) 0.7499(7) 0.4506(3) 0.055(3) Uani 1 1 d G U . . .
H32 H 0.0769 0.7423 0.4264 0.065 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
Cr1 Cl1A 2.71(2) . ?
Cr1 Cl2A 2.09(2) . ?
Cr1 O1 1.974(11) . ?
Cr1 O1 2.000(11) 6_454 ?
Cr1 N1 2.057(13) . ?
Cr1 N2 2.086(12) . ?
Cr1 Cl1 2.321(5) . ?
Cr1 Cl2 2.340(5) . ?
O1 Cr1 2.000(11) 6_454 ?
O1 C6 1.407(16) . ?
N1 C1 1.399(17) . ?
N1 C5 1.366(19) . ?
N2 C7 1.28(2) . ?
N2 C11 1.335(19) . ?
C1 H1 0.9500 . ?
C1 C2 1.41(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.44(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.30(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.38(2) . ?
C5 C6 1.526(16) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.33(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.40(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.34(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.41(2) . ?
C11 H11 0.9500 . ?
Cr2 Cl3A 2.187(8) . ?
Cr2 Cl4A 2.471(8) . ?
Cr2 O2 1.966(13) 6_554 ?
Cr2 O2 1.977(12) . ?
Cr2 N3 2.070(13) . ?
Cr2 N4 2.086(12) . ?
Cr2 Cl3 2.464(9) . ?
Cr2 Cl4 2.208(9) . ?
O2 Cr2 1.966(13) 6_554 ?
O2 C17 1.59(2) . ?
N3 C12 1.34(2) . ?
N3 C16 1.27(2) . ?
N4 C18 1.28(2) . ?
N4 C22 1.32(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.36(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.36(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.39(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.35(3) . ?
C16 C17 1.61(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18 0.9500 . ?
C18 C19 1.42(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.28(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.39(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.34(3) . ?
C22 H22 0.9500 . ?
N5 C23 1.3900 . ?
N5 C27 1.3900 . ?
C23 H23 0.9500 . ?
C23 C24 1.3900 . ?
C24 H24 0.9500 . ?
C24 C25 1.3900 . ?
C25 H25 0.9500 . ?
C25 C26 1.3900 . ?
C26 H26 0.9500 . ?
C26 C27 1.3900 . ?
C27 H27 0.9500 . ?
N6 C28 1.3900 . ?
N6 C32 1.3900 . ?
C28 H28 0.9500 . ?
C28 C29 1.3900 . ?
C29 H29 0.9500 . ?
C29 C30 1.3900 . ?
C30 H30 0.9500 . ?
C30 C31 1.3900 . ?
C31 H31 0.9500 . ?
C31 C32 1.3900 . ?
C32 H32 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
Cl2A Cr1 Cl1A 93.4(10) . . ?
O1 Cr1 Cl1A 73.7(7) . . ?
O1 Cr1 Cl1A 151.7(6) 6_454 . ?
O1 Cr1 Cl2A 165.1(9) . . ?
O1 Cr1 Cl2A 114.5(9) 6_454 . ?
O1 Cr1 O1 79.1(5) . 6_454 ?
O1 Cr1 N1 94.5(5) 6_454 . ?
O1 Cr1 N1 80.7(5) . . ?
O1 Cr1 N2 97.4(5) . . ?
O1 Cr1 N2 89.0(5) 6_454 . ?
O1 Cr1 Cl1 93.7(4) . . ?
O1 Cr1 Cl1 172.4(4) 6_454 . ?
O1 Cr1 Cl2 168.3(4) . . ?
O1 Cr1 Cl2 92.6(4) 6_454 . ?
N1 Cr1 Cl1A 89.1(6) . . ?
N1 Cr1 Cl2A 91.8(6) . . ?
N1 Cr1 N2 175.6(5) . . ?
N1 Cr1 Cl1 87.0(4) . . ?
N1 Cr1 Cl2 91.7(4) . . ?
N2 Cr1 Cl1A 86.6(6) . . ?
N2 Cr1 Cl2A 89.2(7) . . ?
N2 Cr1 Cl1 89.2(4) . . ?
N2 Cr1 Cl2 90.8(4) . . ?
Cl1 Cr1 Cl2 94.8(2) . . ?
Cr1 O1 Cr1 100.6(5) . 6_454 ?
C6 O1 Cr1 122.3(8) . 6_454 ?
C6 O1 Cr1 111.5(8) . . ?
C1 N1 Cr1 129.9(10) . . ?
C5 N1 Cr1 111.6(10) . . ?
C5 N1 C1 118.0(13) . . ?
C7 N2 Cr1 119.8(11) . . ?
C7 N2 C11 118.6(13) . . ?
C11 N2 Cr1 121.4(11) . . ?
N1 C1 H1 119.6 . . ?
N1 C1 C2 120.7(15) . . ?
C2 C1 H1 119.6 . . ?
C1 C2 H2 121.5 . . ?
C1 C2 C3 117.0(15) . . ?
C3 C2 H2 121.5 . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(16) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 119.2 . . ?
C3 C4 C5 121.5(16) . . ?
C5 C4 H4 119.2 . . ?
N1 C5 C4 121.6(14) . . ?
N1 C5 C6 113.9(11) . . ?
C4 C5 C6 124.4(13) . . ?
O1 C6 C5 111.7(10) . . ?
O1 C6 H6A 109.3 . . ?
O1 C6 H6B 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N2 C7 H7 118.8 . . ?
N2 C7 C8 122.4(16) . . ?
C8 C7 H7 118.8 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.8(17) . . ?
C9 C8 H8 119.6 . . ?
C8 C9 H9 120.8 . . ?
C10 C9 C8 118.5(17) . . ?
C10 C9 H9 120.8 . . ?
C9 C10 H10 122.1 . . ?
C9 C10 C11 115.9(16) . . ?
C11 C10 H10 122.1 . . ?
N2 C11 C10 123.2(14) . . ?
N2 C11 H11 118.4 . . ?
C10 C11 H11 118.4 . . ?
Cl3A Cr2 Cl4A 92.5(3) . . ?
O2 Cr2 Cl3A 103.9(5) 6_554 . ?
O2 Cr2 Cl3A 175.1(5) . . ?
O2 Cr2 Cl4A 84.7(5) . . ?
O2 Cr2 Cl4A 162.5(5) 6_554 . ?
O2 Cr2 O2 79.3(6) 6_554 . ?
O2 Cr2 N3 95.2(5) 6_554 . ?
O2 Cr2 N3 82.7(5) . . ?
O2 Cr2 N4 83.9(6) 6_554 . ?
O2 Cr2 N4 97.4(5) . . ?
O2 Cr2 Cl3 84.2(5) 6_554 . ?
O2 Cr2 Cl3 161.7(5) . . ?
O2 Cr2 Cl4 175.6(5) 6_554 . ?
O2 Cr2 Cl4 104.9(5) . . ?
N3 Cr2 Cl3A 93.3(4) . . ?
N3 Cr2 Cl4A 89.6(4) . . ?
N3 Cr2 N4 179.1(5) . . ?
N3 Cr2 Cl3 91.0(5) . . ?
N3 Cr2 Cl4 86.7(5) . . ?
N4 Cr2 Cl3A 86.7(4) . . ?
N4 Cr2 Cl4A 91.3(5) . . ?
N4 Cr2 Cl3 88.7(5) . . ?
N4 Cr2 Cl4 94.1(5) . . ?
Cl4 Cr2 Cl3 91.8(4) . . ?
Cr2 O2 Cr2 100.7(6) 6_554 . ?
C17 O2 Cr2 128.3(10) . 6_554 ?
C17 O2 Cr2 97.3(10) . . ?
C12 N3 Cr2 122.4(12) . . ?
C16 N3 Cr2 121.1(14) . . ?
C16 N3 C12 116.5(17) . . ?
C18 N4 Cr2 121.5(12) . . ?
C18 N4 C22 119.8(16) . . ?
C22 N4 Cr2 118.3(12) . . ?
N3 C12 H12 117.7 . . ?
N3 C12 C13 124.5(19) . . ?
C13 C12 H12 117.7 . . ?
C12 C13 H13 121.8 . . ?
C12 C13 C14 116.5(19) . . ?
C14 C13 H13 121.8 . . ?
C13 C14 H14 120.4 . . ?
C13 C14 C15 119.2(17) . . ?
C15 C14 H14 120.4 . . ?
C14 C15 H15 121.1 . . ?
C16 C15 C14 117.7(18) . . ?
C16 C15 H15 121.1 . . ?
N3 C16 C15 125(2) . . ?
N3 C16 C17 100.2(17) . . ?
C15 C16 C17 134.9(18) . . ?
O2 C17 C16 120.9(16) . . ?
O2 C17 H17A 107.1 . . ?
O2 C17 H17B 107.1 . . ?
C16 C17 H17A 107.1 . . ?
C16 C17 H17B 107.1 . . ?
H17A C17 H17B 106.8 . . ?
N4 C18 H18 119.8 . . ?
N4 C18 C19 120.4(19) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.7(19) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 120.4 . . ?
C19 C20 C21 119.2(18) . . ?
C21 C20 H20 120.4 . . ?
C20 C21 H21 120.9 . . ?
C22 C21 C20 118(2) . . ?
C22 C21 H21 120.9 . . ?
N4 C22 C21 122(2) . . ?
N4 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
C23 N5 C27 120.0 . . ?
N5 C23 H23 120.0 . . ?
N5 C23 C24 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
N5 C27 H27 120.0 . . ?
C26 C27 N5 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 N6 C32 120.0 . . ?
N6 C28 H28 120.0 . . ?
N6 C28 C29 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 H30 120.0 . . ?
C31 C30 C29 120.0 . . ?
C31 C30 H30 120.0 . . ?
C30 C31 H31 120.0 . . ?
C30 C31 C32 120.0 . . ?
C32 C31 H31 120.0 . . ?
N6 C32 H32 120.0 . . ?
C31 C32 N6 120.0 . . ?
C31 C32 H32 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C6 C5 -88.2(11) 6_454 . . . ?
Cr1 O1 C6 C5 30.7(12) . . . . ?
Cr1 N1 C1 C2 -167.6(13) . . . . ?
Cr1 N1 C5 C4 170.1(12) . . . . ?
Cr1 N1 C5 C6 -12.8(14) . . . . ?
Cr1 N2 C7 C8 -176.3(14) . . . . ?
Cr1 N2 C11 C10 170.3(12) . . . . ?
N1 C1 C2 C3 -2(2) . . . . ?
N1 C5 C6 O1 -11.2(15) . . . . ?
N2 C7 C8 C9 7(3) . . . . ?
C1 N1 C5 C4 -3(2) . . . . ?
C1 N1 C5 C6 174.6(12) . . . . ?
C1 C2 C3 C4 0(3) . . . . ?
C2 C3 C4 C5 1(3) . . . . ?
C3 C4 C5 N1 0(2) . . . . ?
C3 C4 C5 C6 -176.5(15) . . . . ?
C4 C5 C6 O1 165.8(13) . . . . ?
C5 N1 C1 C2 3(2) . . . . ?
C7 N2 C11 C10 -5(2) . . . . ?
C7 C8 C9 C10 -7(3) . . . . ?
C8 C9 C10 C11 1(3) . . . . ?
C9 C10 C11 N2 5(3) . . . . ?
C11 N2 C7 C8 0(3) . . . . ?
Cr2 O2 C17 C16 71(2) 6_554 . . . ?
Cr2 O2 C17 C16 -38.5(18) . . . . ?
Cr2 N3 C12 C13 170.9(15) . . . . ?
Cr2 N3 C16 C15 -166.9(18) . . . . ?
Cr2 N3 C16 C17 19(2) . . . . ?
Cr2 N4 C18 C19 171.3(17) . . . . ?
Cr2 N4 C22 C21 -176.7(19) . . . . ?
N3 C12 C13 C14 3(3) . . . . ?
N3 C16 C17 O2 15(2) . . . . ?
N4 C18 C19 C20 -1(4) . . . . ?
C12 N3 C16 C15 12(3) . . . . ?
C12 N3 C16 C17 -162.5(15) . . . . ?
C12 C13 C14 C15 -1(3) . . . . ?
C13 C14 C15 C16 4(3) . . . . ?
C14 C15 C16 N3 -10(4) . . . . ?
C14 C15 C16 C17 161(2) . . . . ?
C15 C16 C17 O2 -158(2) . . . . ?
C16 N3 C12 C13 -8(3) . . . . ?
C18 N4 C22 C21 -5(4) . . . . ?
C18 C19 C20 C21 7(4) . . . . ?
C19 C20 C21 C22 -11(4) . . . . ?
C20 C21 C22 N4 11(4) . . . . ?
C22 N4 C18 C19 0(3) . . . . ?
N5 C23 C24 C25 0.0 . . . . ?
C23 N5 C27 C26 0.0 . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C26 C27 N5 0.0 . . . . ?
C27 N5 C23 C24 0.0 . . . . ?
N6 C28 C29 C30 0.0 . . . . ?
C28 N6 C32 C31 0.0 . . . . ?
C28 C29 C30 C31 0.0 . . . . ?
C29 C30 C31 C32 0.0 . . . . ?
C30 C31 C32 N6 0.0 . . . . ?
C32 N6 C28 C29 0.0 . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-29
_olex2_date_sample_submission    2016-04-25
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id 589
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.909
_oxdiff_exptl_absorpt_empirical_full_min 0.651
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.41(3)
2 0.097(19)
3 0.089(19)
4 0.400(19)

_vrf_PLAT341_5                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02427 Ang.  
RESPONSE: Please see the _refine_special_details section of the CIF.
;
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1482837'
_audit_update_record             
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
# local name eb15267
_audit_creation_date             2015-11-04
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H13 Cl2 Cr N2 O2'
_chemical_formula_sum            'C14 H16 Cl2 Cr N3 O2'
_chemical_formula_weight         381.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C12 H12 Cl2 Cr N2 O2 '
_chemical_oxdiff_usercomment     '@ 120 K 156'
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'
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'
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           133
_space_group_name_H-M_alt        'P 42/n b c'
_space_group_name_Hall           '-P 4ac 2b'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x, z+1/2'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z+1/2'
'x, -y+1/2, -z'
'-x+1/2, y, -z'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z-1/2'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z-1/2'
'-x, y-1/2, z'
'x-1/2, -y, z'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   15.4761(3)
_cell_length_b                   15.4761(3)
_cell_length_c                   12.3453(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2956.82(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    24294
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.1690
_cell_measurement_theta_min      3.7150
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of acetonitrile and diethyl ether by vapour diffusion'
_exptl_crystal_size_max          0.2229
_exptl_crystal_size_mid          0.0507
_exptl_crystal_size_min          0.0432
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            134457
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.107
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -92.00  -51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  173.0000  -53.1619 41

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000  150.0000 51

#__ type_ start__ end____ width___ exp.time_
  3 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000   60.0000 51

#__ type_ start__ end____ width___ exp.time_
  4 omega  -73.00  -32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  140.0000 -123.8148 41

#__ type_ start__ end____ width___ exp.time_
  5 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000  120.0000 51

#__ type_ start__ end____ width___ exp.time_
  6 omega  -68.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -19.0000   60.0000 116

#__ type_ start__ end____ width___ exp.time_
  7 omega  -59.00   37.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -57.0000    0.0000 96

#__ type_ start__ end____ width___ exp.time_
  8 omega  -12.00   83.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372   38.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
  9 omega   13.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -145.0000 -131.5234 65

#__ type_ start__ end____ width___ exp.time_
 10 omega  -62.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -38.0000 -180.0000 95

#__ type_ start__ end____ width___ exp.time_
 11 omega  -66.00  -25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  127.0000   39.2654 41

#__ type_ start__ end____ width___ exp.time_
 12 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000 -150.0000 51

#__ type_ start__ end____ width___ exp.time_
 13 omega  -83.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -77.0000    0.0000 105

#__ type_ start__ end____ width___ exp.time_
 14 omega   -5.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -117.0000   62.3225 66

#__ type_ start__ end____ width___ exp.time_
 15 omega  -16.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372   57.0000  -60.0000 97

#__ type_ start__ end____ width___ exp.time_
 16 omega    4.00   68.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -128.0000  -32.3956 64

#__ type_ start__ end____ width___ exp.time_
 17 omega    6.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -131.0000 -111.6368 64

#__ type_ start__ end____ width___ exp.time_
 18 omega  -20.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -99.0000  -90.0000 71

#__ type_ start__ end____ width___ exp.time_
 19 omega  -20.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000   30.0000 51

#__ type_ start__ end____ width___ exp.time_
 20 omega  -62.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -38.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
 21 omega    9.00   73.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -137.0000  112.1175 64

#__ type_ start__ end____ width___ exp.time_
 22 omega    3.00   67.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -127.0000  -67.2231 64

#__ type_ start__ end____ width___ exp.time_
 23 omega    6.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -131.0000 -179.0000 64

#__ type_ start__ end____ width___ exp.time_
 24 omega   10.00   57.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -138.0000    4.0000 47

#__ type_ start__ end____ width___ exp.time_
 25 omega    6.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372 -130.0000   14.0926 63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0258217000
_diffrn_orient_matrix_UB_12      -0.0374303000
_diffrn_orient_matrix_UB_13      0.0072672000
_diffrn_orient_matrix_UB_21      -0.0369078000
_diffrn_orient_matrix_UB_22      -0.0264181000
_diffrn_orient_matrix_UB_23      -0.0079844000
_diffrn_orient_matrix_UB_31      0.0085227000
_diffrn_orient_matrix_UB_32      -0.0010413000
_diffrn_orient_matrix_UB_33      -0.0564241000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1516
_reflns_number_total             1520
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0489
_refine_ls_restrained_S_all      1.330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0319P)²+7.2479P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1087
_refine_special_details          
;The SQUEEZE routine of PLATON was used to remove electron density corresponding to one MeCN per asymmetric unit which lies on and is disordered along a rotation axis and could not be modelled adequately. The O-bound H atom was assigned an occupancy of 0.5, consistent with disordered within the O1-H1...O1A hydrogen bond and for reasons of charge balance.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
906_ALERT_3_C Large K value in the Analysis of Variance ......      6.472 Check
#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          4 Note
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.1848 Check
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       7.25 Why ?
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
173_ALERT_4_G The CIF-Embedded .res File Contains DANG Records          2 Report
300_ALERT_4_G Atom Site Occupancy of *H1     is Constrained at        0.5 Check
605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        190 A**3
789_ALERT_4_G Atoms with Negative _atom_site_disorder_group  #          1 Check
860_ALERT_3_G Number of Least-Squares Restraints .............          3 Note
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
910_ALERT_3_G Missing # of FCF Reflection(s) Below Th(Min) ...          2 Report
961_ALERT_5_G Dataset Contains no Negative Intensities .......     Please Check

Not significant.

#===============================================================================, SQUEEZE
;

# start Validation Reply Form
_vrf_CHEMW03_8                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: SQUEEZE used, as outlined in the _refine_special_details section of the CIF.
;
# end Validation Reply Form

# SQUEEZE RESULTS (Version =  11015)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.250 -0.004 193 45 ' '
2 0.750 0.750 -0.004 193 45 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 0 1.861
0 2 0 2.632
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          'MeCN removed'


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 C6-H1
 1.888082 with sigma of 0.02
 Cr1-H1
 2.650777 with sigma of 0.02
3. Others
 Fixed Sof: H1(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3), C4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.7500 0.08545(4) 0.0000 0.0155(2) Uani 1 2 d DS T P . .
Cl1 Cl 0.73990(5) -0.01699(5) 0.13715(6) 0.0221(2) Uani 1 1 d . . . . .
O1 O 0.72739(13) 0.17585(14) 0.10813(17) 0.0175(5) Uani 1 1 d D . . . .
H1 H 0.747(2) 0.2272(15) 0.117(4) 0.026 Uiso 0.5 1 d DR . . A -1
N1 N 0.61661(16) 0.09893(16) -0.0141(2) 0.0170(5) Uani 1 1 d . . . . .
C1 C 0.5649(2) 0.0697(2) -0.0941(3) 0.0206(6) Uani 1 1 d . . . . .
H1A H 0.5898 0.0389 -0.1529 0.025 Uiso 1 1 calc R . . . .
C2 C 0.4764(2) 0.0833(2) -0.0928(3) 0.0234(7) Uani 1 1 d . . . . .
H2 H 0.4415 0.0634 -0.1510 0.028 Uiso 1 1 calc R . . . .
C3 C 0.4394(2) 0.1260(2) -0.0064(3) 0.0248(7) Uani 1 1 d . . . . .
H3 H 0.3786 0.1348 -0.0036 0.030 Uiso 1 1 calc R . . . .
C4 C 0.4917(2) 0.1558(2) 0.0758(3) 0.0231(7) Uani 1 1 d . . . . .
H4 H 0.4675 0.1853 0.1361 0.028 Uiso 1 1 calc R . . . .
C5 C 0.5803(2) 0.1420(2) 0.0691(3) 0.0184(6) Uani 1 1 d . . . . .
C6 C 0.6426(2) 0.1726(2) 0.1529(3) 0.0212(7) Uani 1 1 d D . . . .
H6A H 0.6255 0.2308 0.1784 0.025 Uiso 1 1 calc R . . . .
H6B H 0.6417 0.1329 0.2157 0.025 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
Cr1 Cl1 2.3248(9) 6_655 ?
Cr1 Cl1 2.3248(9) . ?
Cr1 O1 1.965(2) 6_655 ?
Cr1 O1 1.965(2) . ?
Cr1 N1 2.082(3) 6_655 ?
Cr1 N1 2.082(3) . ?
O1 H1 0.855(9) . ?
O1 C6 1.425(4) . ?
N1 C1 1.349(4) . ?
N1 C5 1.347(4) . ?
C1 H1A 0.9500 . ?
C1 C2 1.385(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(4) . ?
C5 C6 1.491(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 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
Cl1 Cr1 Cl1 94.01(4) 6_655 . ?
O1 Cr1 Cl1 172.84(6) 6_655 . ?
O1 Cr1 Cl1 172.85(6) . 6_655 ?
O1 Cr1 Cl1 88.78(7) . . ?
O1 Cr1 Cl1 88.78(7) 6_655 6_655 ?
O1 Cr1 O1 89.22(13) . 6_655 ?
O1 Cr1 N1 78.99(9) 6_655 6_655 ?
O1 Cr1 N1 92.77(9) . 6_655 ?
O1 Cr1 N1 78.99(9) . . ?
O1 Cr1 N1 92.78(9) 6_655 . ?
N1 Cr1 Cl1 93.59(7) . . ?
N1 Cr1 Cl1 93.59(7) 6_655 6_655 ?
N1 Cr1 Cl1 94.25(7) 6_655 . ?
N1 Cr1 Cl1 94.24(7) . 6_655 ?
N1 Cr1 N1 168.51(14) . 6_655 ?
Cr1 O1 H1 133.0(18) . . ?
C6 O1 Cr1 113.74(17) . . ?
C6 O1 H1 107.8(17) . . ?
C1 N1 Cr1 128.0(2) . . ?
C5 N1 Cr1 113.5(2) . . ?
C5 N1 C1 118.5(3) . . ?
N1 C1 H1A 119.1 . . ?
N1 C1 C2 121.8(3) . . ?
C2 C1 H1A 119.1 . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.0(3) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 122.1(3) . . ?
N1 C5 C6 114.7(3) . . ?
C4 C5 C6 123.2(3) . . ?
O1 C6 C5 109.7(2) . . ?
O1 C6 H6A 109.7 . . ?
O1 C6 H6B 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O1 0.855(9) 1.557(17) 2.399(4) 168(6) 3_655

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C6 C5 -33.5(3) . . . . ?
Cr1 N1 C1 C2 179.9(2) . . . . ?
Cr1 N1 C5 C4 -178.4(2) . . . . ?
Cr1 N1 C5 C6 1.1(3) . . . . ?
N1 C1 C2 C3 -1.7(5) . . . . ?
N1 C5 C6 O1 20.2(4) . . . . ?
C1 N1 C5 C4 1.1(4) . . . . ?
C1 N1 C5 C6 -179.4(3) . . . . ?
C1 C2 C3 C4 1.4(5) . . . . ?
C2 C3 C4 C5 0.1(5) . . . . ?
C3 C4 C5 N1 -1.4(5) . . . . ?
C3 C4 C5 C6 179.2(3) . . . . ?
C4 C5 C6 O1 -160.3(3) . . . . ?
C5 N1 C1 C2 0.4(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5 4 0 0.0283 5.0000 4.0001 0.0000 -0.0206 -0.2902 0.0384
1 -1 -5 0.1039 1.0000 -1.0000 -5.0000 0.0269 0.0294 0.2917
-1 1 5 0.1025 -1.0000 1.0000 5.0000 -0.0269 -0.0294 -0.2917
-3 5 0 0.0214 -3.0000 5.0000 0.0000 -0.2646 -0.0214 -0.0308
1 0 0 0.0299 1.0000 0.0000 0.0000 0.0258 -0.0369 0.0085
2 -5 0 0.0181 2.0000 -5.0000 -0.0000 0.2388 0.0583 0.0223
-5 -2 0 0.0183 -5.0000 -2.0000 -0.0000 -0.0542 0.2374 -0.0405

_olex2_date_sample_data_collection 2015-11-03
_olex2_date_sample_submission    2015-10-09
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 156
_olex2_submission_special_instructions 'No special instructions were received'


# end of cif
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1482836'
_audit_update_record             
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
# local name eb15261
_audit_creation_date             2015-10-08
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H20 Cl4 Cr2 N2 O4, 2(C2 H3 N)'
_chemical_formula_sum            'C18 H26 Cl4 Cr2 N4 O4'
_chemical_formula_weight         608.23
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cr Cl B Na'
_chemical_oxdiff_usercomment     '@ 120 K 152'
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'
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'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2906(3)
_cell_length_b                   8.5467(3)
_cell_length_c                   10.1679(4)
_cell_angle_alpha                112.400(4)
_cell_angle_beta                 101.243(3)
_cell_angle_gamma                102.099(3)
_cell_volume                     620.49(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5690
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      73.2890
_cell_measurement_theta_min      4.9160
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             310
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of acetonitrile and hexane by vapour diffusion'
_exptl_crystal_size_max          0.0925
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.0399
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10079
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.392
_diffrn_reflns_theta_min         4.938
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00   29.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  120.0000 79

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   29.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -90.0000 79

#__ type_ start__ end____ width___ exp.time_
  3 omega -122.00   -6.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -19.0000  -60.0000 116

#__ type_ start__ end____ width___ exp.time_
  4 omega   12.00  117.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686   77.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
  5 omega   27.00  101.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -130.0000  142.0000 74

#__ type_ start__ end____ width___ exp.time_
  6 omega   23.00   98.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686 -125.0000 -150.0000 75

#__ type_ start__ end____ width___ exp.time_
  7 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 59

#__ type_ start__ end____ width___ exp.time_
  8 omega   30.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -120.0000 79

#__ type_ start__ end____ width___ exp.time_
  9 omega   41.00  139.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  150.0000 98

#__ type_ start__ end____ width___ exp.time_
 10 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 59

#__ type_ start__ end____ width___ exp.time_
 11 omega   40.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -130.0000  142.0000 84

#__ type_ start__ end____ width___ exp.time_
 12 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  120.0000 55

#__ type_ start__ end____ width___ exp.time_
 13 omega   40.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -150.0000 59

#__ type_ start__ end____ width___ exp.time_
 14 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   60.0000 91

#__ type_ start__ end____ width___ exp.time_
 15 omega   94.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 16 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -120.0000 55

#__ type_ start__ end____ width___ exp.time_
 17 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 82

#__ type_ start__ end____ width___ exp.time_
 18 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -150.0000 82

#__ type_ start__ end____ width___ exp.time_
 19 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000    0.0000 91

#__ type_ start__ end____ width___ exp.time_
 20 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 82

#__ type_ start__ end____ width___ exp.time_
 21 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000  120.0000 91

#__ type_ start__ end____ width___ exp.time_
 22 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
 23 omega   37.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
 24 omega   36.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   60.0000 55

#__ type_ start__ end____ width___ exp.time_
 25 omega   39.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -120.0000 82

#__ type_ start__ end____ width___ exp.time_
 26 omega -117.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000   60.0000 105

#__ type_ start__ end____ width___ exp.time_
 27 omega -113.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000  120.0000 96

#__ type_ start__ end____ width___ exp.time_
 28 omega -113.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000 -150.0000 96

#__ type_ start__ end____ width___ exp.time_
 29 omega -117.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000  -30.0000 105

#__ type_ start__ end____ width___ exp.time_
 30 omega    1.00   83.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000    0.0000 82

#__ type_ start__ end____ width___ exp.time_
 31 omega   87.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -60.0000 41

#__ type_ start__ end____ width___ exp.time_
 32 omega   87.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000 -120.0000 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0690679000
_diffrn_orient_matrix_UB_12      -0.0880201000
_diffrn_orient_matrix_UB_13      -0.1718058000
_diffrn_orient_matrix_UB_21      -0.0237423000
_diffrn_orient_matrix_UB_22      0.1758822000
_diffrn_orient_matrix_UB_23      0.0047308000
_diffrn_orient_matrix_UB_31      0.1856334000
_diffrn_orient_matrix_UB_32      0.0588079000
_diffrn_orient_matrix_UB_33      -0.0071201000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2421
_reflns_number_total             2577
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0050(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0837P)²+0.3629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1287
_refine_special_details          
;
O-bound H atoms were located in a difference Fourier map and refined as riding with geometric restraints.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
975_ALERT_2_C Check Calcd Residual Density  0.64A From      O2       0.42 eA-3
#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          3 Note
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
173_ALERT_4_G The CIF-Embedded .res File Contains DANG Records          1 Report
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  Cl1     ..       10.0 su
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  O2      ..        6.1 su
790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          2 Note
              C2 H3 N
860_ALERT_3_G Number of Least-Squares Restraints .............          3 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         40 Note
#===============================================================================


None of the above are significant

;



_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2A = O2-H2B
 0.84 with sigma of 0.02
 H2A-H2B
 1.35 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.44409(5) 0.49478(5) 0.63330(5) 0.02465(19) Uani 1 1 d . . . . .
Cl1 Cl 0.72778(9) 0.62765(10) 0.79609(8) 0.0367(2) Uani 1 1 d . . . . .
Cl2 Cl 0.38542(11) 0.28321(9) 0.72119(9) 0.0376(2) Uani 1 1 d . . . . .
O1 O 0.4747(2) 0.6429(2) 0.5293(2) 0.0267(4) Uani 1 1 d . . . . .
O2 O 0.1929(3) 0.3656(3) 0.4893(2) 0.0307(4) Uani 1 1 d D . . . .
H2A H 0.159(5) 0.266(3) 0.473(4) 0.037 Uiso 1 1 d DR . . . .
H2B H 0.195(5) 0.378(5) 0.417(3) 0.037 Uiso 1 1 d DR . . . .
N1 N 0.3601(3) 0.6782(3) 0.7857(3) 0.0286(5) Uani 1 1 d . . . . .
C1 C 0.3877(4) 0.6893(4) 0.9255(3) 0.0323(6) Uani 1 1 d . . . . .
H1 H 0.4462 0.6152 0.9502 0.039 Uiso 1 1 calc R . . . .
C2 C 0.3347(4) 0.8037(4) 1.0329(4) 0.0365(7) Uani 1 1 d . . . . .
H2 H 0.3544 0.8065 1.1291 0.044 Uiso 1 1 calc R . . . .
C3 C 0.2523(4) 0.9143(4) 0.9988(4) 0.0381(7) Uani 1 1 d . . . . .
H3 H 0.2137 0.9938 1.0706 0.046 Uiso 1 1 calc R . . . .
C4 C 0.2274(4) 0.9068(4) 0.8574(4) 0.0360(7) Uani 1 1 d . . . . .
H4 H 0.1726 0.9831 0.8324 0.043 Uiso 1 1 calc R . . . .
C5 C 0.2819(4) 0.7881(4) 0.7519(3) 0.0300(6) Uani 1 1 d . . . . .
C6 C 0.2587(4) 0.7839(4) 0.6002(3) 0.0315(6) Uani 1 1 d . . . . .
H6A H 0.2164 0.8835 0.5992 0.038 Uiso 1 1 calc R . . . .
H6B H 0.1688 0.6713 0.5254 0.038 Uiso 1 1 calc R . . . .
C7 C 0.4234(4) 0.7978(4) 0.5544(4) 0.0307(6) Uani 1 1 d . . . . .
H7A H 0.4038 0.8145 0.4621 0.037 Uiso 1 1 calc R . . . .
H7B H 0.5176 0.9034 0.6340 0.037 Uiso 1 1 calc R . . . .
N2 N 0.1016(4) -0.0036(4) 0.3528(4) 0.0451(7) Uani 1 1 d . . . . .
C8 C 0.0557(4) -0.1547(4) 0.2837(4) 0.0381(7) Uani 1 1 d . . . . .
C9 C -0.0044(5) -0.3448(5) 0.1935(5) 0.0502(9) Uani 1 1 d . . . . .
H9A H -0.0691 -0.4030 0.2423 0.075 Uiso 1 1 calc GR . . . .
H9B H 0.0950 -0.3877 0.1817 0.075 Uiso 1 1 calc GR . . . .
H9C H -0.0801 -0.3730 0.0951 0.075 Uiso 1 1 calc GR . . . .


_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 Cl1 2.3433(8) . ?
Cr1 Cl2 2.3103(8) . ?
Cr1 O1 1.944(2) . ?
Cr1 O1 1.963(2) 2_666 ?
Cr1 O2 2.077(2) . ?
Cr1 N1 2.091(2) . ?
O1 Cr1 1.963(2) 2_666 ?
O1 C7 1.421(3) . ?
O2 H2A 0.775(18) . ?
O2 H2B 0.784(18) . ?
N1 C1 1.357(4) . ?
N1 C5 1.355(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.377(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.381(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(4) . ?
C5 C6 1.502(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.522(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N2 C8 1.142(4) . ?
C8 C9 1.441(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?

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
Cl2 Cr1 Cl1 92.22(3) . . ?
O1 Cr1 Cl1 90.88(6) 2_666 . ?
O1 Cr1 Cl1 94.26(6) . . ?
O1 Cr1 Cl2 171.24(6) . . ?
O1 Cr1 Cl2 97.01(6) 2_666 . ?
O1 Cr1 O1 77.02(8) . 2_666 ?
O1 Cr1 O2 88.04(9) . . ?
O1 Cr1 O2 88.20(8) 2_666 . ?
O1 Cr1 N1 90.94(9) . . ?
O1 Cr1 N1 167.95(9) 2_666 . ?
O2 Cr1 Cl1 177.27(6) . . ?
O2 Cr1 Cl2 85.34(7) . . ?
O2 Cr1 N1 90.91(9) . . ?
N1 Cr1 Cl1 90.53(7) . . ?
N1 Cr1 Cl2 94.89(7) . . ?
Cr1 O1 Cr1 102.98(8) . 2_666 ?
C7 O1 Cr1 129.69(18) . 2_666 ?
C7 O1 Cr1 126.67(18) . . ?
Cr1 O2 H2A 113(3) . . ?
Cr1 O2 H2B 105(3) . . ?
H2A O2 H2B 113(4) . . ?
C1 N1 Cr1 118.39(19) . . ?
C5 N1 Cr1 122.9(2) . . ?
C5 N1 C1 118.7(2) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.7(3) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.5 . . ?
C1 C2 C3 119.1(3) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.6(3) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.4(3) . . ?
C5 C4 H4 119.8 . . ?
N1 C5 C4 120.5(3) . . ?
N1 C5 C6 119.2(2) . . ?
C4 C5 C6 120.2(3) . . ?
C5 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
C5 C6 C7 113.8(2) . . ?
H6A C6 H6B 107.7 . . ?
C7 C6 H6A 108.8 . . ?
C7 C6 H6B 108.8 . . ?
O1 C7 C6 111.5(2) . . ?
O1 C7 H7A 109.3 . . ?
O1 C7 H7B 109.3 . . ?
C6 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
N2 C8 C9 178.6(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A N2 0.775(18) 2.05(2) 2.777(4) 156(4) .
O2 H2B Cl1 0.784(18) 2.36(2) 3.117(2) 161(4) 2_666

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C7 C6 -33.2(3) . . . . ?
Cr1 O1 C7 C6 135.9(2) 2_666 . . . ?
Cr1 N1 C1 C2 -178.9(2) . . . . ?
Cr1 N1 C5 C4 179.5(2) . . . . ?
Cr1 N1 C5 C6 -2.0(4) . . . . ?
N1 C1 C2 C3 -1.1(5) . . . . ?
N1 C5 C6 C7 -50.1(4) . . . . ?
C1 N1 C5 C4 -1.6(4) . . . . ?
C1 N1 C5 C6 176.9(3) . . . . ?
C1 C2 C3 C4 -0.5(5) . . . . ?
C2 C3 C4 C5 1.0(5) . . . . ?
C3 C4 C5 N1 0.0(5) . . . . ?
C3 C4 C5 C6 -178.4(3) . . . . ?
C4 C5 C6 C7 128.4(3) . . . . ?
C5 N1 C1 C2 2.2(4) . . . . ?
C5 C6 C7 O1 68.4(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 -1 6 0.0167 -1.0005 -0.9998 5.9999 -0.8737 -0.1237 -0.2872
1 1 -6 0.0270 1.0005 0.9998 -5.9999 0.8737 0.1237 0.2872
-5 -1 1 0.0239 -4.9985 -1.0017 1.0015 0.2613 -0.0528 -0.9939
5 1 -1 0.0239 4.9985 1.0017 -1.0015 -0.2613 0.0528 0.9939
1 -6 2 0.0411 1.0009 -6.0015 2.0011 0.1153 -1.0699 -0.1814
5 2 -3 0.0199 4.9986 2.0018 -3.0016 -0.0058 0.2192 1.0670
-5 -2 3 0.0199 -4.9986 -2.0018 3.0016 0.0058 -0.2192 -1.0670
-1 5 -1 0.0313 -1.0009 5.0013 -1.0009 -0.1991 0.8987 0.1154
0 3 3 0.0235 -0.0013 3.0015 2.9989 -0.7793 0.5421 0.1549

_olex2_date_sample_submission    2015-10-07
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 152
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1482832'
_audit_update_record             
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
# local name ro15047
_audit_creation_date             2015-07-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C26 H22 Cr2 N4 O10, 0.5(C H4 O), 0.5 (C4 H10 O)'
_chemical_formula_sum            'C28.50 H29 Cr2 N4 O11'
_chemical_formula_weight         707.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N5 O20 Cr'
_chemical_oxdiff_usercomment     '@ 120 K 860 Ether'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   12.2931(8)
_cell_length_b                   21.3092(16)
_cell_length_c                   13.2192(8)
_cell_angle_alpha                90
_cell_angle_beta                 106.939(7)
_cell_angle_gamma                90
_cell_volume                     3312.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6609
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      24.3220
_cell_measurement_theta_min      3.3440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_recrystallization_method 
'Vapour diffusion from diethyl ether and methanol.'
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.0927
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            47599
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.222
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000   30.0000 53

#__ type_ start__ end____ width___ exp.time_
  3 omega  -20.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -99.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
  4 omega  -47.00   20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.2352  -57.0000   30.0000 67

#__ type_ start__ end____ width___ exp.time_
  5 omega  -63.00   -6.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -38.0000  150.0000 57

#__ type_ start__ end____ width___ exp.time_
  6 omega  -42.00  -16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -38.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
  7 omega  -24.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196   19.0000  120.0000 101

#__ type_ start__ end____ width___ exp.time_
  8 omega   20.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196   38.0000  -30.0000 51

#__ type_ start__ end____ width___ exp.time_
  9 omega   47.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196   38.0000  150.0000 30

#__ type_ start__ end____ width___ exp.time_
 10 omega  -32.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -38.0000 -150.0000 63

#__ type_ start__ end____ width___ exp.time_
 11 omega    8.00   38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        8.7196  -99.0000 -120.0000 30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0041860000
_diffrn_orient_matrix_UB_12      0.0330259000
_diffrn_orient_matrix_UB_13      -0.0067847000
_diffrn_orient_matrix_UB_21      -0.0399259000
_diffrn_orient_matrix_UB_22      0.0011085000
_diffrn_orient_matrix_UB_23      0.0293626000
_diffrn_orient_matrix_UB_31      0.0450073000
_diffrn_orient_matrix_UB_32      0.0040586000
_diffrn_orient_matrix_UB_33      0.0472953000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4892
_reflns_number_total             5824
_reflns_odcompleteness_completeness 98.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         5824
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0830
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0689P)²+17.7889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2129
_refine_special_details          
;
The coordinates of AVARUK from the CSD were used to solve the structure. The solvent molecules exhibit large displacment ellipsoids but disorder could not be modelled. The methanol molecule was modelled as half occupied. The ether molecule was refined as disordered by symmetry over two sites such that there is half an ether per asymmetric unit. The ether molecule was modelled isotropically and H atoms could not be added. They are included in the overall chemical formula, however, and this causes checkCIF errors, which should be ignored.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
216_ALERT_3_B Disordered C29     (An/Solv) ADP max/min Ratio          7.6

See above
#
415_ALERT_2_B Short Inter D-H..H-X       H2     ..  H11     ..       1.92 Ang.


Close approach of disordered components
#===============================================================================
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
043_ALERT_1_C Calculated and Reported Mol. Weight Differ by ..      10.09 Check
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check

Some H atoms could not be added.

341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0097 Ang.
415_ALERT_2_C Short Inter D-H..H-X       H1     ..  H11     ..       2.11 Ang.
430_ALERT_2_C Short Inter D...A Contact  O6     ..  O12B    ..       2.89 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......     10.333 Check
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.473 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Th(Min) ...         10 Report
913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1 Note


Noted.  Data quality as below.
#===============================================================================

#-------------------------------------------------------------------------------

INTENSITY STATISTICS FOR DATASET # 1  RO15047.hkl

 Resolution  #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma

 Inf - 3.05     122    136     89.7     6.09     863.1   45.59  0.0254  0.0120
3.05 - 2.08     283    283    100.0     8.87     383.2   28.80  0.0424  0.0210
2.08 - 1.64     416    416    100.0     9.40     292.6   23.81  0.0550  0.0261
1.64 - 1.44     399    399    100.0    10.20     223.5   19.91  0.0706  0.0336
1.44 - 1.30     424    424    100.0    11.22     151.9   16.04  0.0944  0.0418
1.30 - 1.21     391    391    100.0    11.24     123.5   14.25  0.1109  0.0488
1.21 - 1.14     395    395    100.0    10.76      82.0   10.88  0.1452  0.0635
1.14 - 1.08     423    423    100.0     8.81      72.7    8.98  0.1539  0.0795
1.08 - 1.03     427    427    100.0     8.28      61.6    7.88  0.1780  0.0947
1.03 - 0.99     423    423    100.0     7.79      55.4    7.13  0.1909  0.1072
0.99 - 0.96     347    347    100.0     7.28      58.7    6.91  0.1866  0.1105
0.96 - 0.93     401    401    100.0     6.59      60.1    6.05  0.1973  0.1231
0.93 - 0.90     456    456    100.0     5.76      45.5    4.76  0.2417  0.1716
0.90 - 0.87     514    514    100.0     5.11      47.0    4.26  0.2325  0.1899
0.87 - 0.85     397    397    100.0     4.93      41.0    3.82  0.2543  0.2158
0.85 - 0.83     426    426    100.0     4.68      33.1    3.19  0.3131  0.2606
0.83 - 0.81     448    472     94.9     3.50      26.5    2.39  0.3513  0.3521
0.81 - 0.80     229    262     87.4     2.41      23.0    1.97  0.3663  0.4414
0.80 - 0.78     455    540     84.3     1.95      24.6    1.71  0.3975  0.4668
0.78 - 0.76     410    587     69.8     1.29      22.7    1.47  0.3653  0.5643
0.76 - 0.74     313    855     36.6     0.52      19.0    1.08  0.3735  0.7350
#------------------------------------------------------------------------------
0.84 - 0.74    2071   2932     70.6     1.90      24.9    1.92  0.3481  0.4527
 Inf - 0.74    8099   8974     90.2     6.04     100.5    9.10  0.1012  0.0814

Merged [A],  lowest resolution =  6.40 Angstroms                              

#-------------------------------------------------------------------------------
;

_vrf_PLAT216_1                   
;
PROBLEM: Disordered C29     (An/Solv) ADP max/min Ratio          7.6       
RESPONSE: Please see the _refine_special_details section of the CIF.
;


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O11-C27
 1.5 with sigma of 0.02
 O12A-C28 \\sim O12B-C28 \\sim O12B-C30 \\sim O12A-C30
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O11, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O12A, O12B, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O11(0.5) H11(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
 O12A(0.25) O12B(0.25) C28(0.5) C29(0.5) C30(0.5) C31(0.5)
5.a Riding coordinates:
 O11(H11)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.48642(7) 0.30270(5) 0.46552(7) 0.0236(3) Uani 1 1 d . . . . .
Cr2 Cr 0.68735(7) 0.31580(5) 0.37813(7) 0.0240(3) Uani 1 1 d . . . . .
O1 O 0.5714(3) 0.3157(2) 0.6147(3) 0.0308(10) Uani 1 1 d . . . . .
O2 O 0.6035(4) 0.2782(3) 0.7788(4) 0.0480(13) Uani 1 1 d . . . . .
O3 O 0.3803(3) 0.2903(2) 0.3242(3) 0.0302(10) Uani 1 1 d . . . . .
O4 O 0.2346(4) 0.3346(3) 0.2033(4) 0.0487(13) Uani 1 1 d . . . . .
O5 O 0.7602(3) 0.38803(19) 0.3318(3) 0.0265(9) Uani 1 1 d . . . . .
O6 O 0.9008(3) 0.4576(2) 0.3802(3) 0.0298(10) Uani 1 1 d . . . . .
O7 O 0.7901(3) 0.2538(2) 0.3471(3) 0.0315(10) Uani 1 1 d . . . . .
O8 O 0.8113(5) 0.1841(3) 0.2292(5) 0.0573(15) Uani 1 1 d . . . . .
O9 O 0.6037(3) 0.25229(19) 0.4318(3) 0.0275(9) Uani 1 1 d . . . . .
O10 O 0.5679(3) 0.36714(18) 0.4095(3) 0.0249(9) Uani 1 1 d . . . . .
N1 N 0.4222(4) 0.2303(2) 0.5317(4) 0.0280(11) Uani 1 1 d . . . . .
N2 N 0.3585(4) 0.3624(2) 0.4756(4) 0.0261(11) Uani 1 1 d . . . . .
N3 N 0.8086(4) 0.3366(2) 0.5195(4) 0.0233(10) Uani 1 1 d . . . . .
N4 N 0.6047(4) 0.3003(3) 0.2217(4) 0.0293(12) Uani 1 1 d . . . . .
C1 C 0.3436(6) 0.1875(3) 0.4826(5) 0.0342(15) Uani 1 1 d . . . . .
H1 H 0.3069 0.1918 0.4090 0.041 Uiso 1 1 calc R . . . .
C2 C 0.3153(6) 0.1375(3) 0.5367(6) 0.0456(18) Uani 1 1 d . . . . .
H2 H 0.2604 0.1076 0.5005 0.055 Uiso 1 1 calc R . . . .
C3 C 0.3674(7) 0.1316(4) 0.6432(6) 0.048(2) Uani 1 1 d . . . . .
H3 H 0.3499 0.0971 0.6814 0.058 Uiso 1 1 calc R . . . .
C4 C 0.4451(6) 0.1762(3) 0.6942(6) 0.0404(17) Uani 1 1 d . . . . .
H4 H 0.4801 0.1736 0.7684 0.049 Uiso 1 1 calc R . . . .
C5 C 0.4717(5) 0.2247(3) 0.6362(5) 0.0306(14) Uani 1 1 d . . . . .
C6 C 0.5559(5) 0.2757(3) 0.6830(5) 0.0330(15) Uani 1 1 d . . . . .
C7 C 0.3488(5) 0.3947(3) 0.5587(5) 0.0267(13) Uani 1 1 d . . . . .
H7 H 0.4064 0.3910 0.6243 0.032 Uiso 1 1 calc R . . . .
C8 C 0.2568(5) 0.4338(3) 0.5517(5) 0.0343(15) Uani 1 1 d . . . . .
H8 H 0.2495 0.4551 0.6126 0.041 Uiso 1 1 calc R . . . .
C9 C 0.1764(5) 0.4413(3) 0.4560(6) 0.0395(16) Uani 1 1 d . . . . .
H9 H 0.1136 0.4686 0.4494 0.047 Uiso 1 1 calc R . . . .
C10 C 0.1875(5) 0.4090(3) 0.3696(6) 0.0382(16) Uani 1 1 d . . . . .
H10 H 0.1328 0.4141 0.3025 0.046 Uiso 1 1 calc R . . . .
C11 C 0.2784(5) 0.3694(3) 0.3810(5) 0.0304(14) Uani 1 1 d . . . . .
C12 C 0.2961(5) 0.3289(3) 0.2937(5) 0.0351(15) Uani 1 1 d . . . . .
C13 C 0.8297(5) 0.3083(3) 0.6125(5) 0.0290(14) Uani 1 1 d . . . . .
H13 H 0.7829 0.2742 0.6201 0.035 Uiso 1 1 calc R . . . .
C14 C 0.9179(5) 0.3270(3) 0.6987(5) 0.0346(15) Uani 1 1 d . . . . .
H14 H 0.9321 0.3055 0.7643 0.041 Uiso 1 1 calc R . . . .
C15 C 0.9851(6) 0.3772(3) 0.6887(5) 0.0388(16) Uani 1 1 d . . . . .
H15 H 1.0447 0.3914 0.7476 0.047 Uiso 1 1 calc R . . . .
C16 C 0.9642(5) 0.4065(3) 0.5915(5) 0.0313(14) Uani 1 1 d . . . . .
H16 H 1.0100 0.4407 0.5822 0.038 Uiso 1 1 calc R . . . .
C17 C 0.8759(5) 0.3853(3) 0.5085(4) 0.0257(13) Uani 1 1 d . . . . .
C18 C 0.8457(5) 0.4138(3) 0.3991(4) 0.0243(13) Uani 1 1 d . . . . .
C19 C 0.5139(6) 0.3299(4) 0.1588(5) 0.0393(17) Uani 1 1 d . . . . .
H19 H 0.4742 0.3594 0.1889 0.047 Uiso 1 1 calc R . . . .
C20 C 0.4765(6) 0.3186(4) 0.0507(6) 0.051(2) Uani 1 1 d . . . . .
H20 H 0.4124 0.3403 0.0072 0.061 Uiso 1 1 calc R . . . .
C21 C 0.5337(7) 0.2753(4) 0.0074(6) 0.055(2) Uani 1 1 d . . . . .
H21 H 0.5102 0.2674 -0.0666 0.067 Uiso 1 1 calc R . . . .
C22 C 0.6246(6) 0.2437(4) 0.0721(6) 0.048(2) Uani 1 1 d . . . . .
H22 H 0.6633 0.2128 0.0440 0.058 Uiso 1 1 calc R . . . .
C23 C 0.6590(5) 0.2574(3) 0.1774(5) 0.0353(16) Uani 1 1 d . . . . .
C24 C 0.7616(6) 0.2277(3) 0.2548(6) 0.0407(17) Uani 1 1 d . . . . .
C25 C 0.6288(6) 0.1875(3) 0.4506(5) 0.0359(15) Uani 1 1 d . . . . .
H25A H 0.6731 0.1813 0.5246 0.054 Uiso 1 1 calc GR . . . .
H25B H 0.6730 0.1728 0.4043 0.054 Uiso 1 1 calc GR . . . .
H25C H 0.5578 0.1636 0.4358 0.054 Uiso 1 1 calc GR . . . .
C26 C 0.5750(7) 0.4312(3) 0.4347(7) 0.053(2) Uani 1 1 d . . . . .
H26A H 0.6309 0.4375 0.5039 0.079 Uiso 1 1 calc GR . . . .
H26B H 0.5004 0.4463 0.4371 0.079 Uiso 1 1 calc GR . . . .
H26C H 0.5985 0.4546 0.3808 0.079 Uiso 1 1 calc GR . . . .
O11 O 0.6371(18) 0.4144(9) 0.8155(12) 0.142(8) Uani 0.5 1 d D U P . .
H11 H 0.6921 0.3826 0.8509 0.213 Uiso 0.5 1 d R . P . .
C27 C 0.6801(19) 0.4517(10) 0.7477(14) 0.107(8) Uani 0.5 1 d D U P . .
H27A H 0.6833 0.4956 0.7704 0.160 Uiso 0.5 1 calc GR . P . .
H27B H 0.6302 0.4480 0.6751 0.160 Uiso 0.5 1 calc GR . P . .
H27C H 0.7567 0.4374 0.7506 0.160 Uiso 0.5 1 calc GR . P . .
O12A O 0.719(3) 0.5353(16) 0.025(2) 0.129(10) Uani 0.25 1 d D U P A 2
O12B O 0.818(3) 0.5253(17) 0.183(2) 0.131(10) Uani 0.25 1 d D U P A 1
C28 C 0.859(3) 0.5285(10) 0.0744(17) 0.110(7) Uani 0.5 1 d D U P . .
C29 C 0.959(6) 0.5151(12) 0.003(5) 0.27(3) Uani 0.5 1 d . U P A -1
C30 C 0.680(3) 0.5323(11) 0.133(2) 0.118(8) Uani 0.5 1 d D U P . .
C31 C 0.614(5) 0.563(3) 0.166(3) 0.25(3) Uani 0.5 1 d . U P A -1


_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 O1 1.963(4) . ?
Cr1 O3 1.960(4) . ?
Cr1 O9 1.951(4) . ?
Cr1 O10 1.967(4) . ?
Cr1 N1 2.043(5) . ?
Cr1 N2 2.058(5) . ?
Cr2 O5 1.966(4) . ?
Cr2 O7 1.951(4) . ?
Cr2 O9 1.954(4) . ?
Cr2 O10 1.969(4) . ?
Cr2 N3 2.071(5) . ?
Cr2 N4 2.047(5) . ?
O1 C6 1.295(8) . ?
O2 C6 1.232(8) . ?
O3 C12 1.293(8) . ?
O4 C12 1.220(8) . ?
O5 C18 1.286(7) . ?
O6 C18 1.221(7) . ?
O7 C24 1.293(8) . ?
O8 C24 1.213(8) . ?
O9 C25 1.421(8) . ?
O10 C26 1.402(8) . ?
N1 C1 1.349(8) . ?
N1 C5 1.343(8) . ?
N2 C7 1.331(8) . ?
N2 C11 1.356(8) . ?
N3 C13 1.325(8) . ?
N3 C17 1.361(8) . ?
N4 C19 1.340(9) . ?
N4 C23 1.361(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.382(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.373(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(11) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(9) . ?
C5 C6 1.504(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.386(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.369(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.373(9) . ?
C11 C12 1.506(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.381(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.375(8) . ?
C17 C18 1.511(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.389(10) . ?
C20 H20 0.9500 . ?
C20 C21 1.382(12) . ?
C21 H21 0.9500 . ?
C21 C22 1.370(12) . ?
C22 H22 0.9500 . ?
C22 C23 1.363(9) . ?
C23 C24 1.512(10) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O11 H11 0.9747 . ?
O11 C27 1.412(17) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O12A C28 1.65(2) . ?
O12A C30 1.64(2) . ?
O12B C28 1.65(2) . ?
O12B C30 1.65(2) . ?
C28 C29 1.78(5) . ?
C30 C31 1.22(5) . ?

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
O1 Cr1 O10 95.72(17) . . ?
O1 Cr1 N1 80.52(19) . . ?
O1 Cr1 N2 92.33(18) . . ?
O3 Cr1 O1 171.05(17) . . ?
O3 Cr1 O10 90.30(17) . . ?
O3 Cr1 N1 94.22(19) . . ?
O3 Cr1 N2 80.59(18) . . ?
O9 Cr1 O1 95.43(17) . . ?
O9 Cr1 O3 92.22(17) . . ?
O9 Cr1 O10 78.88(17) . . ?
O9 Cr1 N1 94.87(18) . . ?
O9 Cr1 N2 170.15(18) . . ?
O10 Cr1 N1 172.44(18) . . ?
O10 Cr1 N2 94.34(18) . . ?
N1 Cr1 N2 92.38(19) . . ?
O5 Cr2 O10 93.77(17) . . ?
O5 Cr2 N3 80.79(17) . . ?
O5 Cr2 N4 87.09(18) . . ?
O7 Cr2 O5 94.76(17) . . ?
O7 Cr2 O9 92.80(17) . . ?
O7 Cr2 O10 171.05(17) . . ?
O7 Cr2 N3 89.71(18) . . ?
O7 Cr2 N4 80.78(19) . . ?
O9 Cr2 O5 172.31(17) . . ?
O9 Cr2 O10 78.74(16) . . ?
O9 Cr2 N3 97.87(18) . . ?
O9 Cr2 N4 95.52(19) . . ?
O10 Cr2 N3 94.34(17) . . ?
O10 Cr2 N4 96.95(19) . . ?
N4 Cr2 N3 163.93(19) . . ?
C6 O1 Cr1 117.7(4) . . ?
C12 O3 Cr1 117.5(4) . . ?
C18 O5 Cr2 118.3(4) . . ?
C24 O7 Cr2 118.4(4) . . ?
Cr1 O9 Cr2 101.75(19) . . ?
C25 O9 Cr1 129.3(4) . . ?
C25 O9 Cr2 128.7(4) . . ?
Cr1 O10 Cr2 100.61(18) . . ?
C26 O10 Cr1 126.4(4) . . ?
C26 O10 Cr2 126.4(4) . . ?
C1 N1 Cr1 128.0(4) . . ?
C5 N1 Cr1 113.0(4) . . ?
C5 N1 C1 118.8(6) . . ?
C7 N2 Cr1 128.9(4) . . ?
C7 N2 C11 119.3(5) . . ?
C11 N2 Cr1 111.8(4) . . ?
C13 N3 Cr2 129.4(4) . . ?
C13 N3 C17 119.1(5) . . ?
C17 N3 Cr2 111.5(4) . . ?
C19 N4 Cr2 129.0(5) . . ?
C19 N4 C23 118.3(5) . . ?
C23 N4 Cr2 112.4(4) . . ?
N1 C1 H1 119.2 . . ?
N1 C1 C2 121.6(7) . . ?
C2 C1 H1 119.2 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.3(7) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.2(7) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(7) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.8(6) . . ?
N1 C5 C6 114.2(5) . . ?
C4 C5 C6 123.9(6) . . ?
O1 C6 C5 114.3(5) . . ?
O2 C6 O1 124.5(6) . . ?
O2 C6 C5 121.1(6) . . ?
N2 C7 H7 119.2 . . ?
N2 C7 C8 121.6(6) . . ?
C8 C7 H7 119.2 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.1(6) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.4(6) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.4(6) . . ?
C11 C10 H10 120.3 . . ?
N2 C11 C10 121.2(6) . . ?
N2 C11 C12 114.6(5) . . ?
C10 C11 C12 124.2(6) . . ?
O3 C12 C11 114.1(5) . . ?
O4 C12 O3 125.4(6) . . ?
O4 C12 C11 120.6(6) . . ?
N3 C13 H13 119.1 . . ?
N3 C13 C14 121.9(6) . . ?
C14 C13 H13 119.1 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.4(6) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 120.5 . . ?
C14 C15 C16 119.0(6) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 120.6 . . ?
C17 C16 C15 118.8(6) . . ?
C17 C16 H16 120.6 . . ?
N3 C17 C16 121.9(5) . . ?
N3 C17 C18 114.9(5) . . ?
C16 C17 C18 123.2(6) . . ?
O5 C18 C17 114.4(5) . . ?
O6 C18 O5 125.1(5) . . ?
O6 C18 C17 120.5(5) . . ?
N4 C19 H19 119.3 . . ?
N4 C19 C20 121.5(7) . . ?
C20 C19 H19 119.3 . . ?
C19 C20 H20 120.4 . . ?
C21 C20 C19 119.2(7) . . ?
C21 C20 H20 120.4 . . ?
C20 C21 H21 120.4 . . ?
C22 C21 C20 119.3(7) . . ?
C22 C21 H21 120.4 . . ?
C21 C22 H22 120.4 . . ?
C23 C22 C21 119.2(7) . . ?
C23 C22 H22 120.4 . . ?
N4 C23 C22 122.5(7) . . ?
N4 C23 C24 114.0(5) . . ?
C22 C23 C24 123.5(7) . . ?
O7 C24 C23 113.6(6) . . ?
O8 C24 O7 125.0(7) . . ?
O8 C24 C23 121.3(7) . . ?
O9 C25 H25A 109.5 . . ?
O9 C25 H25B 109.5 . . ?
O9 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O10 C26 H26A 109.5 . . ?
O10 C26 H26B 109.5 . . ?
O10 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 O11 H11 111.1 . . ?
O11 C27 H27A 109.5 . . ?
O11 C27 H27B 109.5 . . ?
O11 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C30 O12A C28 101(2) . . ?
C30 O12B C28 101(2) . . ?
O12B C28 C29 152(3) . . ?
C31 C30 O12B 129(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C6 O2 180.0(5) . . . . ?
Cr1 O1 C6 C5 -0.9(6) . . . . ?
Cr1 O3 C12 O4 166.7(5) . . . . ?
Cr1 O3 C12 C11 -12.5(7) . . . . ?
Cr1 N1 C1 C2 174.3(5) . . . . ?
Cr1 N1 C5 C4 -175.9(5) . . . . ?
Cr1 N1 C5 C6 4.8(6) . . . . ?
Cr1 N2 C7 C8 179.3(4) . . . . ?
Cr1 N2 C11 C10 -177.7(5) . . . . ?
Cr1 N2 C11 C12 4.3(6) . . . . ?
Cr2 O5 C18 O6 177.7(4) . . . . ?
Cr2 O5 C18 C17 -2.1(6) . . . . ?
Cr2 O7 C24 O8 -172.0(6) . . . . ?
Cr2 O7 C24 C23 9.2(7) . . . . ?
Cr2 N3 C13 C14 177.3(4) . . . . ?
Cr2 N3 C17 C16 -178.5(5) . . . . ?
Cr2 N3 C17 C18 1.7(6) . . . . ?
Cr2 N4 C19 C20 172.1(5) . . . . ?
Cr2 N4 C23 C22 -174.3(5) . . . . ?
Cr2 N4 C23 C24 4.4(6) . . . . ?
N1 C1 C2 C3 0.7(10) . . . . ?
N1 C5 C6 O1 -2.7(7) . . . . ?
N1 C5 C6 O2 176.4(6) . . . . ?
N2 C7 C8 C9 -2.8(9) . . . . ?
N2 C11 C12 O3 4.9(8) . . . . ?
N2 C11 C12 O4 -174.3(6) . . . . ?
N3 C13 C14 C15 1.0(10) . . . . ?
N3 C17 C18 O5 0.1(7) . . . . ?
N3 C17 C18 O6 -179.7(5) . . . . ?
N4 C19 C20 C21 0.6(11) . . . . ?
N4 C23 C24 O7 -8.9(8) . . . . ?
N4 C23 C24 O8 172.3(6) . . . . ?
C1 N1 C5 C4 0.6(9) . . . . ?
C1 N1 C5 C6 -178.7(5) . . . . ?
C1 C2 C3 C4 1.2(10) . . . . ?
C2 C3 C4 C5 -2.2(10) . . . . ?
C3 C4 C5 N1 1.3(10) . . . . ?
C3 C4 C5 C6 -179.4(6) . . . . ?
C4 C5 C6 O1 177.9(6) . . . . ?
C4 C5 C6 O2 -2.9(9) . . . . ?
C5 N1 C1 C2 -1.6(9) . . . . ?
C7 N2 C11 C10 -0.1(9) . . . . ?
C7 N2 C11 C12 -178.1(5) . . . . ?
C7 C8 C9 C10 1.4(10) . . . . ?
C8 C9 C10 C11 0.6(10) . . . . ?
C9 C10 C11 N2 -1.3(10) . . . . ?
C9 C10 C11 C12 176.5(6) . . . . ?
C10 C11 C12 O3 -173.0(6) . . . . ?
C10 C11 C12 O4 7.8(10) . . . . ?
C11 N2 C7 C8 2.2(9) . . . . ?
C13 N3 C17 C16 -1.0(8) . . . . ?
C13 N3 C17 C18 179.3(5) . . . . ?
C13 C14 C15 C16 -1.7(10) . . . . ?
C14 C15 C16 C17 1.1(10) . . . . ?
C15 C16 C17 N3 0.3(9) . . . . ?
C15 C16 C17 C18 -180.0(6) . . . . ?
C16 C17 C18 O5 -179.6(5) . . . . ?
C16 C17 C18 O6 0.5(9) . . . . ?
C17 N3 C13 C14 0.3(9) . . . . ?
C19 N4 C23 C22 0.1(9) . . . . ?
C19 N4 C23 C24 178.8(5) . . . . ?
C19 C20 C21 C22 1.2(11) . . . . ?
C20 C21 C22 C23 -2.2(11) . . . . ?
C21 C22 C23 N4 1.6(10) . . . . ?
C21 C22 C23 C24 -177.0(6) . . . . ?
C22 C23 C24 O7 169.8(6) . . . . ?
C22 C23 C24 O8 -9.0(10) . . . . ?
C23 N4 C19 C20 -1.3(9) . . . . ?
C28 O12B C30 C31 -139(4) . . . . ?
C30 O12B C28 C29 -161(4) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3 -5 4 0.0510 -3.0000 -5.0001 4.0000 -0.1797 0.2317 0.0339
3 5 -4 0.0510 3.0000 5.0001 -4.0000 0.1797 -0.2317 -0.0339
5 3 3 0.1161 5.0000 2.9999 3.0000 0.0578 -0.1082 0.3791
-5 -3 -3 0.1161 -5.0000 -2.9999 -3.0000 -0.0578 0.1082 -0.3791
3 1 5 0.1271 3.0000 0.9999 5.0001 -0.0135 0.0281 0.3756
-3 -1 -5 0.1271 -3.0000 -0.9999 -5.0001 0.0135 -0.0281 -0.3756
1 -5 -1 0.0464 1.0000 -5.0000 -1.0000 -0.1625 -0.0748 -0.0226
-1 5 1 0.0464 -1.0000 5.0000 1.0000 0.1625 0.0748 0.0226
4 -5 2 0.1083 4.0000 -5.0000 2.0000 -0.1954 -0.1065 0.2543
-4 5 -2 0.1083 -4.0000 5.0000 -2.0000 0.1954 0.1065 -0.2543
1 5 4 0.1063 1.0000 4.9999 4.0000 0.1338 0.0831 0.2545
-1 -5 -4 0.1063 -1.0000 -4.9999 -4.0000 -0.1338 -0.0831 -0.2545
-5 2 5 0.0460 -5.0000 1.9999 5.0000 0.0531 0.3487 0.0196
5 0 -1 0.1060 5.0000 0.0000 -1.0000 -0.0141 -0.2290 0.1777
1 5 0 0.0704 1.0000 5.0000 -0.0000 0.1609 -0.0344 0.0653

_olex2_date_sample_data_collection 2015-07-23
_olex2_date_sample_submission    2015-07-20
_olex2_exptl_crystal_mounting_method 'Mitegen tip, Paratone oil.'
_olex2_submission_original_sample_id '860 Ether'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1482834'
_audit_update_record             
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
# local name eb15349x2
_audit_creation_date             2015-11-26
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H20 Br2 Cr2 N4 O6'
_chemical_formula_sum            'C24 H20 Br2 Cr2 N4 O6'
_chemical_formula_weight         724.26
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N4 O10 Cr Br'
_chemical_oxdiff_usercomment     '@ 120 K 240o'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           34
_space_group_name_H-M_alt        'P n n 2'
_space_group_name_Hall           'P 2 -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   7.8068(2)
_cell_length_b                   12.2423(4)
_cell_length_c                   13.3916(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1279.88(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4892
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.5150
_cell_measurement_theta_min      4.2070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_recrystallization_method 
'The material was recrystallised from acetonitrile by solvothermal methods'
_exptl_crystal_size_max          0.2406
_exptl_crystal_size_mid          0.0961
_exptl_crystal_size_min          0.0943
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11349
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.769
_diffrn_reflns_theta_min         3.042
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -20.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.2747  -99.0000    0.0000 51

#__ type_ start__ end____ width___ exp.time_
  2 omega  -62.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -38.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
  3 omega  -62.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -38.0000  120.0000 93

#__ type_ start__ end____ width___ exp.time_
  4 omega  -58.00   26.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8372  -57.0000   30.0000 84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0454592000
_diffrn_orient_matrix_UB_12      0.0498867000
_diffrn_orient_matrix_UB_13      -0.0051834000
_diffrn_orient_matrix_UB_21      -0.0137915000
_diffrn_orient_matrix_UB_22      -0.0114767000
_diffrn_orient_matrix_UB_23      -0.0512829000
_diffrn_orient_matrix_UB_31      -0.0774340000
_diffrn_orient_matrix_UB_32      -0.0271752000
_diffrn_orient_matrix_UB_33      0.0121500000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.8
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.825
_reflns_number_gt                3011
_reflns_number_total             3209
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 
;
 Flack x determined using 1252 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0304
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²+0.7893P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0570
_refine_special_details          
;
#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0067 Ang.
915_ALERT_3_C Low Friedel Pair Coverage ......................         83 %

Not significant

#===============================================================================
795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence ..         C1 Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Th(Min) ...          2 Report
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        116 Note
951_ALERT_5_G Calculated (ThMax) and CIF-Reported Kmax Differ           2 Units
957_ALERT_1_G Calculated (ThMax) and Actual (FCF) Kmax Differ           2 Units

Not significant

#===============================================================================

;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Br1 Br 0.56992(4) 0.80100(3) 0.16824(5) 0.01617(10) Uani 1 1 d . . . . .
Cr1 Cr 0.61431(7) 0.60100(5) 0.15724(5) 0.01131(14) Uani 1 1 d . . . . .
O1 O 0.6309(3) 0.4401(2) 0.1613(3) 0.0132(5) Uani 1 1 d . . . . .
O2 O 0.8588(4) 0.6142(2) 0.1282(2) 0.0156(7) Uani 1 1 d . . . . .
O3 O 1.0499(4) 0.6282(3) 0.0040(3) 0.0240(8) Uani 1 1 d . . . . .
N1 N 0.6703(5) 0.5779(3) 0.3072(3) 0.0134(7) Uani 1 1 d . . . . .
N2 N 0.6003(4) 0.6160(3) 0.0054(3) 0.0122(7) Uani 1 1 d . . . . .
C1 C 0.6556(6) 0.6495(4) 0.3830(3) 0.0174(9) Uani 1 1 d . . . . .
H1 H 0.6092 0.7198 0.3699 0.021 Uiso 1 1 calc R . . . .
C2 C 0.7059(6) 0.6243(4) 0.4794(4) 0.0195(10) Uani 1 1 d . . . . .
H2 H 0.6942 0.6762 0.5316 0.023 Uiso 1 1 calc R . . . .
C3 C 0.7735(6) 0.5220(4) 0.4982(3) 0.0228(10) Uani 1 1 d . . . . .
H3 H 0.8089 0.5028 0.5638 0.027 Uiso 1 1 calc R . . . .
C4 C 0.7892(5) 0.4484(4) 0.4215(4) 0.0191(9) Uani 1 1 d . . . . .
H4 H 0.8358 0.3779 0.4335 0.023 Uiso 1 1 calc R . . . .
C5 C 0.7362(5) 0.4778(4) 0.3258(3) 0.0140(9) Uani 1 1 d . . . . .
C6 C 0.7474(5) 0.4037(4) 0.2367(3) 0.0152(9) Uani 1 1 d . . . . .
H6A H 0.8657 0.4041 0.2101 0.018 Uiso 1 1 calc R . . . .
H6B H 0.7186 0.3281 0.2566 0.018 Uiso 1 1 calc R . . . .
C7 C 0.4592(5) 0.6272(4) -0.0516(3) 0.0146(9) Uani 1 1 d . . . . .
H7 H 0.3497 0.6285 -0.0207 0.018 Uiso 1 1 calc R . . . .
C8 C 0.4709(6) 0.6367(4) -0.1544(3) 0.0188(10) Uani 1 1 d . . . . .
H8 H 0.3707 0.6471 -0.1936 0.023 Uiso 1 1 calc R . . . .
C9 C 0.6306(6) 0.6309(4) -0.1994(4) 0.0226(10) Uani 1 1 d . . . . .
H9 H 0.6408 0.6336 -0.2700 0.027 Uiso 1 1 calc R . . . .
C10 C 0.7760(6) 0.6212(4) -0.1398(4) 0.0201(10) Uani 1 1 d . . . . .
H10 H 0.8868 0.6176 -0.1690 0.024 Uiso 1 1 calc R . . . .
C11 C 0.7560(5) 0.6168(4) -0.0379(3) 0.0152(9) Uani 1 1 d . . . . .
C12 C 0.9041(5) 0.6194(4) 0.0351(3) 0.0166(10) Uani 1 1 d . . . . .


_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
Br1 Cr1 2.4773(7) . ?
Cr1 O1 1.975(3) . ?
Cr1 O1 1.980(2) 2_665 ?
Cr1 O2 1.954(3) . ?
Cr1 N1 2.074(4) . ?
Cr1 N2 2.045(4) . ?
O1 Cr1 1.980(2) 2_665 ?
O1 C6 1.430(5) . ?
O2 C12 1.297(5) . ?
O3 C12 1.216(5) . ?
N1 C1 1.346(6) . ?
N1 C5 1.352(6) . ?
N2 C7 1.347(5) . ?
N2 C11 1.346(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.384(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.382(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.372(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.394(6) . ?
C5 C6 1.501(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.385(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.387(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.393(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.375(6) . ?
C11 C12 1.515(6) . ?

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
O1 Cr1 Br1 173.43(10) . . ?
O1 Cr1 Br1 96.56(7) 2_665 . ?
O1 Cr1 O1 79.01(10) . 2_665 ?
O1 Cr1 N1 79.84(15) . . ?
O1 Cr1 N1 98.20(15) 2_665 . ?
O1 Cr1 N2 89.90(15) 2_665 . ?
O1 Cr1 N2 96.92(15) . . ?
O2 Cr1 Br1 93.84(9) . . ?
O2 Cr1 O1 166.03(13) . 2_665 ?
O2 Cr1 O1 91.35(11) . . ?
O2 Cr1 N1 89.92(13) . . ?
O2 Cr1 N2 81.18(13) . . ?
N1 Cr1 Br1 96.13(11) . . ?
N2 Cr1 Br1 87.86(10) . . ?
N2 Cr1 N1 170.48(16) . . ?
Cr1 O1 Cr1 100.90(10) . 2_665 ?
C6 O1 Cr1 123.7(3) . 2_665 ?
C6 O1 Cr1 111.8(2) . . ?
C12 O2 Cr1 117.5(2) . . ?
C1 N1 Cr1 128.6(3) . . ?
C1 N1 C5 118.9(4) . . ?
C5 N1 Cr1 112.5(3) . . ?
C7 N2 Cr1 128.1(3) . . ?
C11 N2 Cr1 112.3(3) . . ?
C11 N2 C7 119.6(4) . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.3(4) . . ?
C2 C1 H1 118.9 . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.7(5) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.5(4) . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.1(4) . . ?
N1 C5 C6 115.0(4) . . ?
C4 C5 C6 123.9(4) . . ?
O1 C6 C5 109.7(3) . . ?
O1 C6 H6A 109.7 . . ?
O1 C6 H6B 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 H7 119.4 . . ?
N2 C7 C8 121.2(4) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 H8 120.5 . . ?
C7 C8 C9 119.1(4) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.2(4) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.7(4) . . ?
C11 C10 H10 120.7 . . ?
N2 C11 C10 122.0(4) . . ?
N2 C11 C12 114.3(4) . . ?
C10 C11 C12 123.6(4) . . ?
O2 C12 C11 114.2(3) . . ?
O3 C12 O2 126.1(4) . . ?
O3 C12 C11 119.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C6 C5 -85.0(4) 2_665 . . . ?
Cr1 O1 C6 C5 35.8(4) . . . . ?
Cr1 O2 C12 O3 179.7(4) . . . . ?
Cr1 O2 C12 C11 1.2(5) . . . . ?
Cr1 N1 C1 C2 -176.8(3) . . . . ?
Cr1 N1 C5 C4 177.1(3) . . . . ?
Cr1 N1 C5 C6 -2.6(4) . . . . ?
Cr1 N2 C7 C8 179.9(3) . . . . ?
Cr1 N2 C11 C10 176.9(4) . . . . ?
Cr1 N2 C11 C12 -6.6(5) . . . . ?
N1 C1 C2 C3 0.0(7) . . . . ?
N1 C5 C6 O1 -21.0(5) . . . . ?
N2 C7 C8 C9 2.2(7) . . . . ?
N2 C11 C12 O2 3.8(6) . . . . ?
N2 C11 C12 O3 -174.8(4) . . . . ?
C1 N1 C5 C4 -0.3(6) . . . . ?
C1 N1 C5 C6 180.0(4) . . . . ?
C1 C2 C3 C4 0.0(7) . . . . ?
C2 C3 C4 C5 -0.2(7) . . . . ?
C3 C4 C5 N1 0.3(6) . . . . ?
C3 C4 C5 C6 -180.0(4) . . . . ?
C4 C5 C6 O1 159.2(4) . . . . ?
C5 N1 C1 C2 0.1(6) . . . . ?
C7 N2 C11 C10 -4.5(7) . . . . ?
C7 N2 C11 C12 171.9(4) . . . . ?
C7 C8 C9 C10 -3.2(7) . . . . ?
C8 C9 C10 C11 0.4(7) . . . . ?
C9 C10 C11 N2 3.5(7) . . . . ?
C9 C10 C11 C12 -172.6(4) . . . . ?
C10 C11 C12 O2 -179.8(4) . . . . ?
C10 C11 C12 O3 1.6(7) . . . . ?
C11 N2 C7 C8 1.6(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -12 14 0.0287 -0.0000 -12.0000 14.0000 -0.6712 -0.5802 0.4962
-1 12 -14 0.0579 -1.0000 12.0000 -14.0000 0.7167 0.5940 -0.4188
9 8 -4 0.1033 9.0000 8.0000 -4.0000 0.0107 -0.0108 -0.9629
-10 3 -8 0.0941 -10.0000 3.0000 -8.0000 0.6457 0.5137 0.5956
-1 13 12 0.0364 -1.0000 13.0000 12.0000 0.6318 -0.7508 -0.1300
0 -14 -11 0.0521 -0.0000 -14.0000 -11.0000 -0.6414 0.7248 0.2468
-9 -11 1 0.0934 -9.0000 -11.0000 1.0000 -0.1448 0.1991 1.0080
8 -3 -12 0.0858 8.0000 -3.0000 -12.0000 -0.4511 0.5395 -0.6837
-1 3 -18 0.0640 -1.0000 3.0000 -18.0000 0.2884 0.9025 -0.2228
-8 -4 -11 0.0806 -8.0000 -4.0000 -11.0000 0.2211 0.7204 0.5945
9 6 10 0.1194 9.0000 6.0000 10.0000 -0.1616 -0.7058 -0.7385
0 17 -5 0.0588 0.0000 17.0000 -5.0000 0.8740 0.0613 -0.5227
10 -9 1 0.0970 10.0000 -9.0000 1.0000 -0.9088 -0.0859 -0.5176
-1 -9 -16 0.0531 -1.0000 -9.0000 -16.0000 -0.3206 0.9376 0.1276
1 -17 0 0.0396 1.0000 -17.0000 0.0000 -0.8935 0.1813 0.3845

_olex2_date_sample_submission    2015-11-23
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 240o
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1482835'
_audit_update_record             
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
# local name eb15300
_audit_creation_date             2015-11-06
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 H8 Cl2 Cr N O2), 2(C4 H10 O)'
_chemical_formula_sum            'C20 H36 Cl4 Cr2 N2 O6'
_chemical_formula_weight         646.31
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N8 O20 Cr Cl'
_chemical_oxdiff_usercomment     '@ 120 K 194'
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'
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'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7732(4)
_cell_length_b                   10.4693(3)
_cell_length_c                   14.0067(7)
_cell_angle_alpha                92.473(4)
_cell_angle_beta                 99.099(4)
_cell_angle_gamma                91.960(3)
_cell_volume                     1412.58(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7317
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.1210
_cell_measurement_theta_min      3.4580
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of diethyl ether and acetonitrile by vapour diffusion'
_exptl_crystal_size_max          0.1925
_exptl_crystal_size_mid          0.1588
_exptl_crystal_size_min          0.111
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6514
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.854
_diffrn_reflns_theta_min         3.288
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -78.00   19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -57.0000   30.0000 97

#__ type_ start__ end____ width___ exp.time_
  2 omega  -20.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -99.0000   30.0000 53

#__ type_ start__ end____ width___ exp.time_
  3 omega  -30.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914   38.0000 -150.0000 95

#__ type_ start__ end____ width___ exp.time_
  4 omega  -30.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914   38.0000  120.0000 95

#__ type_ start__ end____ width___ exp.time_
  5 omega  -80.00   15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914  -38.0000   60.0000 95

#__ type_ start__ end____ width___ exp.time_
  6 omega  -20.00   49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        8.8758  -99.0000  -30.0000 69

#__ type_ start__ end____ width___ exp.time_
  7 omega  -30.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -7.3914   38.0000   30.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0650571000
_diffrn_orient_matrix_UB_12      0.0332403000
_diffrn_orient_matrix_UB_13      0.0026154000
_diffrn_orient_matrix_UB_21      -0.0330881000
_diffrn_orient_matrix_UB_22      0.0591741000
_diffrn_orient_matrix_UB_23      0.0011362000
_diffrn_orient_matrix_UB_31      0.0091927000
_diffrn_orient_matrix_UB_32      0.0003376000
_diffrn_orient_matrix_UB_33      0.0512683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5624
_reflns_number_total             6514
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0728
_refine_ls_restrained_S_all      1.265
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+11.0388P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.1652
_refine_special_details          
'The TwinRotMat routine of Platon was used to identify a minor amount of residual non-merohedral twinning and create a two-component reflection file (twin law [-1 0 0 / 0 -1 0 / 0.458 0.130 1] which was used for refinement. Water H atoms were identified in a difference Fourier map and refined as riding with bond distance and 1,3 distance restraints.'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.884(2) 0.116(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O52-H52A = O52-H52B = O2-H2B = O2-H2A
 0.84 with sigma of 0.02
 H2A-H2B = H52B-H52A
 1.35 with sigma of 0.04
4.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C57(H57A,H57B),
 C59(H59A,H59B)
4.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C52(H52), C53(H53), C54(H54), C1(H1), C2(H2), C3(H3), C4(H4)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Cr51 Cr 0.07435(10) 0.91899(8) 0.07736(6) 0.0128(2) Uani 1 1 d . . . . .
Cr1 Cr 0.07170(10) 0.40689(8) 0.44005(6) 0.0135(2) Uani 1 1 d . . . . .
Cl2 Cl -0.13722(15) 0.32967(13) 0.34605(10) 0.0176(3) Uani 1 1 d . . . . .
Cl52 Cl 0.18116(15) 0.93357(14) 0.23585(10) 0.0190(3) Uani 1 1 d . . . . .
Cl51 Cl -0.13166(15) 0.84060(13) 0.12131(10) 0.0175(3) Uani 1 1 d . . . . .
Cl1 Cl 0.18278(16) 0.40344(14) 0.30733(10) 0.0206(3) Uani 1 1 d . . . . .
N51 N 0.1261(5) 0.7366(4) 0.0410(3) 0.0138(9) Uani 1 1 d . . . . .
C51 C 0.1702(6) 0.6454(6) 0.1012(4) 0.0188(12) Uani 1 1 d . . . . .
H51 H 0.1831 0.6642 0.1691 0.023 Uiso 1 1 calc R . . . .
C52 C 0.1974(6) 0.5252(6) 0.0672(4) 0.0188(12) Uani 1 1 d . . . . .
H52 H 0.2299 0.4620 0.1110 0.023 Uiso 1 1 calc R . . . .
C53 C 0.1766(6) 0.4974(6) -0.0320(4) 0.0194(12) Uani 1 1 d . . . . .
H53 H 0.1948 0.4149 -0.0568 0.023 Uiso 1 1 calc R . . . .
C56 C 0.0507(7) 0.8169(5) -0.1190(4) 0.0180(12) Uani 1 1 d . . . . .
H56A H 0.1266 0.8569 -0.1481 0.022 Uiso 1 1 calc R . . . .
H56B H -0.0225 0.7830 -0.1719 0.022 Uiso 1 1 calc R . . . .
C54 C 0.1294(6) 0.5901(5) -0.0939(4) 0.0185(12) Uani 1 1 d . . . . .
H54 H 0.1137 0.5720 -0.1619 0.022 Uiso 1 1 calc R . . . .
C55 C 0.1051(6) 0.7101(5) -0.0565(4) 0.0149(11) Uani 1 1 d . . . . .
O51 O -0.0040(4) 0.9083(4) -0.0593(3) 0.0136(8) Uani 1 1 d . . . . .
N1 N 0.1135(5) 0.2291(4) 0.4877(3) 0.0133(9) Uani 1 1 d . . . . .
C1 C 0.1753(6) 0.1351(6) 0.4425(4) 0.0192(12) Uani 1 1 d . . . . .
H1 H 0.1995 0.1487 0.3806 0.023 Uiso 1 1 calc R . . . .
C2 C 0.2036(7) 0.0212(6) 0.4842(4) 0.0207(13) Uani 1 1 d . . . . .
H2 H 0.2469 -0.0433 0.4513 0.025 Uiso 1 1 calc R . . . .
C5 C 0.0787(6) 0.2090(5) 0.5760(4) 0.0149(11) Uani 1 1 d . . . . .
C6 C 0.0085(7) 0.3169(6) 0.6215(4) 0.0200(12) Uani 1 1 d . . . . .
H6A H -0.0801 0.2845 0.6391 0.024 Uiso 1 1 calc R . . . .
H6B H 0.0685 0.3512 0.6814 0.024 Uiso 1 1 calc R . . . .
O1 O -0.0169(4) 0.4145(4) 0.5560(3) 0.0158(8) Uani 1 1 d . . . . .
O52 O 0.2544(4) 0.9818(4) 0.0363(3) 0.0162(8) Uani 1 1 d D . . . .
C3 C 0.1691(6) -0.0001(6) 0.5746(4) 0.0184(12) Uani 1 1 d . . . . .
H3 H 0.1885 -0.0786 0.6046 0.022 Uiso 1 1 calc R . . . .
C4 C 0.1054(6) 0.0961(5) 0.6204(4) 0.0178(12) Uani 1 1 d . . . . .
H4 H 0.0803 0.0839 0.6823 0.021 Uiso 1 1 calc R . . . .
O2 O 0.2515(4) 0.4714(4) 0.5237(3) 0.0188(9) Uani 1 1 d D . . . .
O3 O 0.4516(5) 0.3388(4) 0.6260(3) 0.0227(9) Uani 1 1 d . . . . .
O53 O 0.4846(5) 1.1118(4) 0.1414(3) 0.0297(11) Uani 1 1 d . . . . .
C7 C 0.4944(7) 0.3930(7) 0.7232(5) 0.0302(15) Uani 1 1 d . . . . .
H7A H 0.5424 0.4774 0.7209 0.036 Uiso 1 1 calc R . . . .
H7B H 0.5599 0.3363 0.7602 0.036 Uiso 1 1 calc R . . . .
C10 C 0.5265(8) 0.2603(8) 0.4796(5) 0.0371(18) Uani 1 1 d . . . . .
H10A H 0.4692 0.3231 0.4439 0.056 Uiso 1 1 calc GR . . . .
H10B H 0.4726 0.1794 0.4786 0.056 Uiso 1 1 calc GR . . . .
H10C H 0.6086 0.2461 0.4491 0.056 Uiso 1 1 calc GR . . . .
C9 C 0.5706(7) 0.3094(7) 0.5817(5) 0.0257(14) Uani 1 1 d . . . . .
H9A H 0.6244 0.2442 0.6187 0.031 Uiso 1 1 calc R . . . .
H9B H 0.6313 0.3874 0.5831 0.031 Uiso 1 1 calc R . . . .
C8 C 0.3702(8) 0.4081(7) 0.7719(5) 0.0320(16) Uani 1 1 d . . . . .
H8A H 0.3102 0.4709 0.7387 0.048 Uiso 1 1 calc GR . . . .
H8B H 0.4001 0.4376 0.8395 0.048 Uiso 1 1 calc GR . . . .
H8C H 0.3189 0.3256 0.7693 0.048 Uiso 1 1 calc GR . . . .
C58 C 0.5451(8) 0.9358(8) 0.2358(6) 0.0377(18) Uani 1 1 d . . . . .
H58A H 0.4615 0.8903 0.2009 0.057 Uiso 1 1 calc GR . . . .
H58B H 0.5646 0.9065 0.3019 0.057 Uiso 1 1 calc GR . . . .
H58C H 0.6238 0.9184 0.2023 0.057 Uiso 1 1 calc GR . . . .
C57 C 0.5232(8) 1.0755(8) 0.2392(5) 0.0388(18) Uani 1 1 d . . . . .
H57A H 0.4489 1.0951 0.2774 0.047 Uiso 1 1 calc R . . . .
H57B H 0.6094 1.1230 0.2698 0.047 Uiso 1 1 calc R . . . .
C59 C 0.4906(10) 1.2471(7) 0.1339(6) 0.048(2) Uani 1 1 d . . . . .
H59A H 0.5774 1.2839 0.1728 0.057 Uiso 1 1 calc R . . . .
H59B H 0.4115 1.2847 0.1596 0.057 Uiso 1 1 calc R . . . .
C60 C 0.4854(9) 1.2787(8) 0.0308(6) 0.044(2) Uani 1 1 d . . . . .
H60A H 0.3936 1.2537 -0.0056 0.065 Uiso 1 1 calc GR . . . .
H60B H 0.5564 1.2323 0.0031 0.065 Uiso 1 1 calc GR . . . .
H60C H 0.5027 1.3710 0.0270 0.065 Uiso 1 1 calc GR . . . .
H2A H 0.321(6) 0.429(7) 0.544(5) 0.052 Uiso 1 1 d DR . . . .
H2B H 0.235(8) 0.519(7) 0.569(4) 0.052 Uiso 1 1 d DR . . . .
H52A H 0.321(6) 1.011(7) 0.076(5) 0.052 Uiso 1 1 d DR . . . .
H52B H 0.223(8) 1.038(5) 0.000(5) 0.052 Uiso 1 1 d DR . . . .


_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
Cr51 Cl52 2.2952(16) . ?
Cr51 Cl51 2.3299(17) . ?
Cr51 N51 2.056(5) . ?
Cr51 O51 1.943(4) . ?
Cr51 O51 1.968(4) 2_575 ?
Cr51 O52 2.034(4) . ?
Cr1 Cl2 2.3453(17) . ?
Cr1 Cl1 2.2958(16) . ?
Cr1 N1 2.037(5) . ?
Cr1 O1 1.957(4) . ?
Cr1 O1 1.963(4) 2_566 ?
Cr1 O2 2.029(4) . ?
N51 C51 1.338(7) . ?
N51 C55 1.363(7) . ?
C51 H51 0.9500 . ?
C51 C52 1.376(8) . ?
C52 H52 0.9500 . ?
C52 C53 1.389(8) . ?
C53 H53 0.9500 . ?
C53 C54 1.372(8) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C55 1.509(8) . ?
C56 O51 1.418(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.383(7) . ?
O51 Cr51 1.968(4) 2_575 ?
N1 C1 1.357(7) . ?
N1 C5 1.357(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.368(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.386(8) . ?
C5 C6 1.511(8) . ?
C5 C4 1.372(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 O1 1.406(7) . ?
O1 Cr1 1.963(4) 2_566 ?
O52 H52A 0.83(2) . ?
O52 H52B 0.83(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(8) . ?
C4 H4 0.9500 . ?
O2 H2A 0.84(2) . ?
O2 H2B 0.83(2) . ?
O3 C7 1.444(8) . ?
O3 C9 1.438(7) . ?
O53 C57 1.433(8) . ?
O53 C59 1.425(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.493(10) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 C9 1.492(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C58 C57 1.485(11) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.489(11) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?

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
Cl52 Cr51 Cl51 91.51(6) . . ?
N51 Cr51 Cl52 98.97(14) . . ?
N51 Cr51 Cl51 90.72(14) . . ?
O51 Cr51 Cl52 176.21(13) . . ?
O51 Cr51 Cl52 102.18(12) 2_575 . ?
O51 Cr51 Cl51 92.78(12) 2_575 . ?
O51 Cr51 Cl51 92.19(12) . . ?
O51 Cr51 N51 80.14(17) . . ?
O51 Cr51 N51 158.45(17) 2_575 . ?
O51 Cr51 O51 78.48(17) . 2_575 ?
O51 Cr51 O52 86.84(16) . . ?
O51 Cr51 O52 88.68(17) 2_575 . ?
O52 Cr51 Cl52 89.44(12) . . ?
O52 Cr51 Cl51 178.05(13) . . ?
O52 Cr51 N51 87.45(18) . . ?
Cl1 Cr1 Cl2 91.64(6) . . ?
N1 Cr1 Cl2 91.30(14) . . ?
N1 Cr1 Cl1 99.89(14) . . ?
O1 Cr1 Cl2 90.60(13) . . ?
O1 Cr1 Cl2 94.49(13) 2_566 . ?
O1 Cr1 Cl1 100.75(12) 2_566 . ?
O1 Cr1 Cl1 177.65(14) . . ?
O1 Cr1 N1 158.38(17) 2_566 . ?
O1 Cr1 N1 80.77(17) . . ?
O1 Cr1 O1 78.36(17) . 2_566 ?
O1 Cr1 O2 88.43(17) . . ?
O1 Cr1 O2 86.06(17) 2_566 . ?
O2 Cr1 Cl2 178.77(14) . . ?
O2 Cr1 Cl1 89.35(13) . . ?
O2 Cr1 N1 87.80(18) . . ?
C51 N51 Cr51 127.4(4) . . ?
C51 N51 C55 119.7(5) . . ?
C55 N51 Cr51 112.8(4) . . ?
N51 C51 H51 119.2 . . ?
N51 C51 C52 121.6(5) . . ?
C52 C51 H51 119.2 . . ?
C51 C52 H52 120.4 . . ?
C51 C52 C53 119.1(5) . . ?
C53 C52 H52 120.4 . . ?
C52 C53 H53 120.3 . . ?
C54 C53 C52 119.4(5) . . ?
C54 C53 H53 120.3 . . ?
H56A C56 H56B 108.5 . . ?
C55 C56 H56A 110.2 . . ?
C55 C56 H56B 110.2 . . ?
O51 C56 H56A 110.2 . . ?
O51 C56 H56B 110.2 . . ?
O51 C56 C55 107.7(4) . . ?
C53 C54 H54 120.3 . . ?
C53 C54 C55 119.4(5) . . ?
C55 C54 H54 120.3 . . ?
N51 C55 C56 116.3(5) . . ?
N51 C55 C54 120.7(5) . . ?
C54 C55 C56 123.0(5) . . ?
Cr51 O51 Cr51 101.52(17) . 2_575 ?
C56 O51 Cr51 117.1(3) . . ?
C56 O51 Cr51 134.5(3) . 2_575 ?
C1 N1 Cr1 127.0(4) . . ?
C1 N1 C5 119.0(5) . . ?
C5 N1 Cr1 114.0(4) . . ?
N1 C1 H1 119.3 . . ?
N1 C1 C2 121.5(5) . . ?
C2 C1 H1 119.3 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 119.9(5) . . ?
C3 C2 H2 120.0 . . ?
N1 C5 C6 116.2(5) . . ?
N1 C5 C4 121.3(5) . . ?
C4 C5 C6 122.5(5) . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
O1 C6 C5 109.7(4) . . ?
O1 C6 H6A 109.7 . . ?
O1 C6 H6B 109.7 . . ?
Cr1 O1 Cr1 101.64(17) . 2_566 ?
C6 O1 Cr1 118.1(3) . . ?
C6 O1 Cr1 137.1(3) . 2_566 ?
Cr51 O52 H52A 122(6) . . ?
Cr51 O52 H52B 99(6) . . ?
H52A O52 H52B 110(5) . . ?
C2 C3 H3 120.8 . . ?
C2 C3 C4 118.4(5) . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 119.9(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
Cr1 O2 H2A 128(6) . . ?
Cr1 O2 H2B 110(6) . . ?
H2A O2 H2B 109(5) . . ?
C9 O3 C7 110.5(5) . . ?
C59 O53 C57 112.2(6) . . ?
O3 C7 H7A 109.8 . . ?
O3 C7 H7B 109.8 . . ?
O3 C7 C8 109.5(6) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
O3 C9 C10 110.4(5) . . ?
O3 C9 H9A 109.6 . . ?
O3 C9 H9B 109.6 . . ?
C10 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
O53 C57 C58 107.4(6) . . ?
O53 C57 H57A 110.2 . . ?
O53 C57 H57B 110.2 . . ?
C58 C57 H57A 110.2 . . ?
C58 C57 H57B 110.2 . . ?
H57A C57 H57B 108.5 . . ?
O53 C59 H59A 109.7 . . ?
O53 C59 H59B 109.7 . . ?
O53 C59 C60 109.9(7) . . ?
H59A C59 H59B 108.2 . . ?
C60 C59 H59A 109.7 . . ?
C60 C59 H59B 109.7 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A O3 0.84(2) 1.89(3) 2.697(6) 161(8) .
O52 H52A O53 0.83(2) 1.96(3) 2.766(6) 165(8) .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr51 N51 C51 C52 177.9(4) . . . . ?
Cr51 N51 C55 C56 0.8(6) . . . . ?
Cr51 N51 C55 C54 -177.6(5) . . . . ?
Cr1 N1 C1 C2 176.9(5) . . . . ?
Cr1 N1 C5 C6 3.3(6) . . . . ?
Cr1 N1 C5 C4 -177.2(4) . . . . ?
N51 C51 C52 C53 -0.9(9) . . . . ?
C51 N51 C55 C56 178.0(5) . . . . ?
C51 N51 C55 C54 -0.3(8) . . . . ?
C51 C52 C53 C54 0.0(9) . . . . ?
C52 C53 C54 C55 0.8(9) . . . . ?
C53 C54 C55 N51 -0.6(9) . . . . ?
C53 C54 C55 C56 -178.8(6) . . . . ?
C55 N51 C51 C52 1.1(9) . . . . ?
C55 C56 O51 Cr51 27.2(6) . . . . ?
C55 C56 O51 Cr51 171.9(4) . . . 2_575 ?
O51 C56 C55 N51 -17.1(7) . . . . ?
O51 C56 C55 C54 161.2(5) . . . . ?
N1 C1 C2 C3 -0.1(9) . . . . ?
N1 C5 C6 O1 5.1(7) . . . . ?
N1 C5 C4 C3 0.0(9) . . . . ?
C1 N1 C5 C6 -179.2(5) . . . . ?
C1 N1 C5 C4 0.3(8) . . . . ?
C1 C2 C3 C4 0.3(9) . . . . ?
C2 C3 C4 C5 -0.3(9) . . . . ?
C5 N1 C1 C2 -0.2(9) . . . . ?
C5 C6 O1 Cr1 -167.4(4) . . . 2_566 ?
C5 C6 O1 Cr1 -11.8(6) . . . . ?
C6 C5 C4 C3 179.4(6) . . . . ?
C4 C5 C6 O1 -174.4(5) . . . . ?
C7 O3 C9 C10 -176.8(6) . . . . ?
C9 O3 C7 C8 -173.2(6) . . . . ?
C57 O53 C59 C60 165.6(7) . . . . ?
C59 O53 C57 C58 -167.1(7) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5 6 -16 0.0933 -5.0001 5.9999 -16.0006 -0.1677 0.5023 -0.8643
-10 10 4 0.0758 -10.0000 10.0000 4.0001 -0.3077 0.9272 0.1165
-3 2 19 0.0883 -2.9999 2.0001 19.0007 -0.0790 0.2392 0.9472
6 -7 14 0.0921 6.0001 -6.9999 14.0006 0.1943 -0.5968 0.7706
11 8 -4 0.0460 11.0001 8.0001 -4.0003 0.9711 0.1049 -0.1013
-2 -1 -19 0.0736 -2.0001 -1.0001 -19.0007 -0.2131 -0.0146 -0.9929
-11 -7 -5 0.0581 -11.0001 -7.0001 -5.0001 -0.9614 -0.0559 -0.3598
-10 -7 12 0.0565 -10.0000 -7.0000 12.0006 -0.8519 -0.0697 0.5210
2 1 19 0.0765 2.0001 1.0001 19.0007 0.2131 0.0146 0.9929
3 -10 -14 0.0626 2.9999 -10.0001 -14.0005 -0.1739 -0.7069 -0.6936
2 -10 14 0.0813 2.0001 -9.9999 14.0006 -0.1657 -0.6420 0.7328
-3 12 11 0.0968 -2.9999 12.0001 11.0004 0.2325 0.8219 0.5404
-4 14 -2 0.0860 -4.0000 14.0000 -2.0002 0.1999 0.9585 -0.1346
-1 -12 -9 0.0565 -1.0001 -12.0001 -9.0003 -0.4875 -0.6872 -0.4747
-2 -13 10 0.0683 -2.0000 -13.0000 10.0005 -0.5361 -0.6917 0.4899
6 -13 0 0.1002 6.0000 -13.0000 0.0001 -0.0418 -0.9678 0.0508

_olex2_date_sample_submission    2015-11-04
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 194
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.884(2)
2 0.116(2)
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1540439'
_audit_update_record             
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
# local name eb16202
_audit_creation_date             2016-08-25
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C12 H13 Cl2 Cr N2 O)'
_chemical_formula_sum            'C24 H26 Cl4 Cr2 N4 O2'
_chemical_formula_weight         648.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     '@ 120 K 679'
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'
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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   14.29325(19)
_cell_length_b                   14.06348(14)
_cell_length_c                   14.8511(2)
_cell_angle_alpha                90
_cell_angle_beta                 117.3958(17)
_cell_angle_gamma                90
_cell_volume                     2650.46(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    23006
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.9260
_cell_measurement_theta_min      3.3310
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.720
_exptl_absorpt_correction_T_max  0.9727
_exptl_absorpt_correction_T_min  0.5795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0953 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.5958.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -4 9 0.0689
2 -9 -1 0.0318
1 9 -3 0.0382
-7 -3 -1 0.0151
7 3 1 0.0151
-2 9 3 0.0594
6 -1 -9 0.1131
-7 2 -2 0.0165
-7 6 4 0.0594

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of 4-picoline and diethyl ether by vapour diffusion'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.0052 -3.9935 8.9993 -0.0647 -0.9822 -0.3065
1.9896 -8.9985 -0.9960 -0.0901 -0.5888 0.8141
1.0095 8.9958 -3.0022 -0.0111 0.8966 -0.5153
-6.9938 -2.9986 -1.0052 0.9341 -0.1683 0.1832
6.9938 2.9986 1.0052 -0.9341 0.1683 -0.1832
-1.9910 8.9995 2.9963 -0.0394 0.4392 -0.9381
5.9980 -1.0055 -8.9962 -0.1282 0.6161 0.7394
-6.9883 1.9995 -2.0068 0.9514 0.2783 -0.1538
-6.9886 6.0017 3.9931 0.5248 0.1270 -0.8452

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43244
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.778
_diffrn_reflns_theta_min         3.142
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  -2.00   1.00    5.00    --  -43.17 125.00 -90.00   94
  2  ω   -113.00 -17.00   1.00    5.00    --  -43.17 -57.00-150.00   96
  3  ω   -116.00 -21.00   1.00    5.00    --  -43.17 -38.00  90.00   95
  4  ω     17.00 113.00   1.00    5.00    --   43.17  57.00  30.00   96
  5  ω     40.00 135.00   1.00   20.00    --  111.00 -45.00-120.00   95
  6  ω     30.00 109.00   1.00   20.00    --  111.00 -94.00-150.00   79
  7  ω     87.00 178.00   1.00   20.00    --  111.00  30.00-180.00   91
  8  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00  30.00  105
  9  ω     30.00 109.00   1.00   20.00    --  111.00 -94.00-120.00   79
 10  ω     87.00 178.00   1.00   20.00    --  111.00  30.00 -90.00   91
 11  ω   -113.00 -17.00   1.00    5.00    --  -43.17 -57.00 -60.00   96
 12  ω    -66.00  29.00   1.00    5.00    --  -43.17  38.00 -90.00   95
 13  ω    -66.00  29.00   1.00    5.00    --  -43.17  38.00-180.00   95
 14  ω     87.00 178.00   1.00   20.00    --  111.00  30.00 120.00   91
 15  ω     80.00 178.00   1.00   20.00    --  111.00  77.00 -60.00   98
 16  ω     83.00 178.00   1.00   20.00    --  111.00  61.00-150.00   95
 17  ω     39.00 121.00   1.00   20.00    --  111.00-125.00  60.00   82
 18  ω     83.00 178.00   1.00   20.00    --  111.00  61.00  60.00   95
 19  ω     66.00 178.00   1.00   20.00    --  111.00  15.00  60.00  112
 20  ω   -117.00 -12.00   1.00    5.00    --  -43.17 -77.00 150.00  105
 21  ω    -66.00  29.00   1.00    5.00    --  -43.17  38.00  90.00   95
 22  ω   -117.00 -12.00   1.00    5.00    --  -43.17 -77.00  60.00  105
 23  ω     83.00 178.00   1.00   20.00    --  111.00  61.00 120.00   95
 24  ω     80.00 178.00   1.00   20.00    --  111.00  77.00   0.00   98
 25  ω     83.00 178.00   1.00   20.00    --  111.00  61.00-180.00   95
 26  ω     30.00 102.00   1.00   20.00    --  111.00 -94.00 120.00   72
 27  ω     83.00 178.00   1.00   20.00    --  111.00  61.00 -30.00   95
 28  ω     83.00 178.00   1.00   20.00    --  111.00  61.00 -90.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1202101000
_diffrn_orient_matrix_UB_12      -0.0093843000
_diffrn_orient_matrix_UB_13      -0.0648485000
_diffrn_orient_matrix_UB_21      0.0029401000
_diffrn_orient_matrix_UB_22      0.0743698000
_diffrn_orient_matrix_UB_23      -0.0748320000
_diffrn_orient_matrix_UB_31      0.0169558000
_diffrn_orient_matrix_UB_32      -0.0798628000
_diffrn_orient_matrix_UB_33      -0.0619545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5054
_reflns_number_total             5513
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5513
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0806P)²+1.2782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1227
_refine_special_details          
;
#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
978_ALERT_2_C Number C-C Bonds with Positive Residual Density           0 Note

Not significant

#===============================================================================
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
142_ALERT_4_G s.u. on b - Axis Small or Missing ..............    0.00014 Ang.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  Cl1     ..        5.0 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  N2      ..        5.9 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr51   --  Cl52    ..        6.0 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr51   --  N52     ..        5.3 s.u.
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         76 Note

Not significant
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C56(H56A,H56B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C51(H51),
 C52(H52), C53(H53), C54(H54), C57(H57), C58(H58), C60(H60), C61(H61)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C62(H62A,H62B,H62C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.10740(3) -0.05414(3) 0.34721(3) 0.03386(13) Uani 1 1 d . . . . .
Cl1 Cl 0.28110(5) -0.04218(5) 0.37681(6) 0.04847(18) Uani 1 1 d . . . . .
Cl2 Cl 0.15325(5) -0.07661(5) 0.51698(5) 0.04629(17) Uani 1 1 d . . . . .
O1 O 0.04809(14) -0.05467(11) 0.19764(14) 0.0356(4) Uani 1 1 d . . . . .
N1 N 0.12141(15) -0.19796(14) 0.32124(16) 0.0367(4) Uani 1 1 d . . . . .
N2 N 0.09800(16) 0.09347(15) 0.36172(16) 0.0382(4) Uani 1 1 d . . . . .
C1 C 0.14394(19) -0.27150(18) 0.3860(2) 0.0402(5) Uani 1 1 d . . . . .
H1 H 0.1500 -0.2604 0.4515 0.048 Uiso 1 1 calc R . . . .
C2 C 0.1586(2) -0.36269(18) 0.3601(2) 0.0443(6) Uani 1 1 d . . . . .
H2 H 0.1742 -0.4132 0.4073 0.053 Uiso 1 1 calc R . . . .
C3 C 0.1504(2) -0.37987(19) 0.2650(2) 0.0462(6) Uani 1 1 d . . . . .
H3 H 0.1602 -0.4421 0.2459 0.055 Uiso 1 1 calc R . . . .
C4 C 0.1275(2) -0.30437(19) 0.1980(2) 0.0440(6) Uani 1 1 d . . . . .
H4 H 0.1207 -0.3142 0.1320 0.053 Uiso 1 1 calc R . . . .
C5 C 0.11473(19) -0.21414(18) 0.2290(2) 0.0380(5) Uani 1 1 d . . . . .
C6 C 0.0928(2) -0.12718(18) 0.1631(2) 0.0414(5) Uani 1 1 d . . . . .
H6A H 0.1592 -0.1040 0.1653 0.050 Uiso 1 1 calc R . . . .
H6B H 0.0435 -0.1436 0.0920 0.050 Uiso 1 1 calc R . . . .
C7 C 0.0404(2) 0.12857(18) 0.4034(2) 0.0424(5) Uani 1 1 d . . . . .
H7 H 0.0047 0.0855 0.4263 0.051 Uiso 1 1 calc R . . . .
C8 C 0.0302(2) 0.22557(19) 0.4149(2) 0.0457(6) Uani 1 1 d . . . . .
H8 H -0.0124 0.2476 0.4443 0.055 Uiso 1 1 calc R . . . .
C9 C 0.0825(2) 0.28997(18) 0.3833(2) 0.0456(6) Uani 1 1 d . . . . .
C10 C 0.1424(2) 0.2526(2) 0.3400(2) 0.0457(6) Uani 1 1 d . . . . .
H10 H 0.1796 0.2940 0.3172 0.055 Uiso 1 1 calc R . . . .
C11 C 0.1479(2) 0.15542(19) 0.3300(2) 0.0432(6) Uani 1 1 d . . . . .
H11 H 0.1887 0.1315 0.2994 0.052 Uiso 1 1 calc R . . . .
C12 C 0.0722(3) 0.3955(2) 0.3940(3) 0.0585(8) Uani 1 1 d . . . . .
H12A H -0.0018 0.4114 0.3726 0.088 Uiso 1 1 calc GR . . . .
H12B H 0.0968 0.4297 0.3513 0.088 Uiso 1 1 calc GR . . . .
H12C H 0.1150 0.4141 0.4650 0.088 Uiso 1 1 calc GR . . . .
Cr51 Cr 0.39210(3) 0.43788(3) 0.25050(3) 0.03207(12) Uani 1 1 d . . . . .
Cl51 Cl 0.21938(5) 0.41606(5) 0.12554(5) 0.04364(16) Uani 1 1 d . . . . .
Cl52 Cl 0.34578(5) 0.45324(4) 0.38056(5) 0.04259(16) Uani 1 1 d . . . . .
O51 O 0.54552(14) 0.43559(11) 0.34492(13) 0.0352(4) Uani 1 1 d . . . . .
N51 N 0.41458(16) 0.29436(14) 0.28767(16) 0.0355(4) Uani 1 1 d . . . . .
N52 N 0.37709(16) 0.58500(15) 0.22089(16) 0.0369(4) Uani 1 1 d . . . . .
C51 C 0.3500(2) 0.22131(18) 0.2393(2) 0.0395(5) Uani 1 1 d . . . . .
H51 H 0.2878 0.2332 0.1780 0.047 Uiso 1 1 calc R . . . .
C52 C 0.3716(2) 0.12962(19) 0.2763(2) 0.0482(6) Uani 1 1 d . . . . .
H52 H 0.3258 0.0788 0.2404 0.058 Uiso 1 1 calc R . . . .
C53 C 0.4614(2) 0.1129(2) 0.3669(3) 0.0514(7) Uani 1 1 d . . . . .
H53 H 0.4767 0.0506 0.3947 0.062 Uiso 1 1 calc R . . . .
C54 C 0.5286(2) 0.1873(2) 0.4164(2) 0.0461(6) Uani 1 1 d . . . . .
H54 H 0.5908 0.1769 0.4781 0.055 Uiso 1 1 calc R . . . .
C55 C 0.5034(2) 0.27739(18) 0.37441(19) 0.0382(5) Uani 1 1 d . . . . .
C56 C 0.5714(2) 0.36336(19) 0.41993(18) 0.0408(5) Uani 1 1 d . . . . .
H56A H 0.5605 0.3876 0.4770 0.049 Uiso 1 1 calc R . . . .
H56B H 0.6466 0.3457 0.4467 0.049 Uiso 1 1 calc R . . . .
C57 C 0.3983(2) 0.65114(19) 0.2924(2) 0.0427(5) Uani 1 1 d . . . . .
H57 H 0.4214 0.6316 0.3605 0.051 Uiso 1 1 calc R . . . .
C58 C 0.3876(2) 0.7477(2) 0.2698(2) 0.0488(6) Uani 1 1 d . . . . .
H58 H 0.4012 0.7927 0.3221 0.059 Uiso 1 1 calc R . . . .
C59 C 0.3573(2) 0.77866(19) 0.1722(3) 0.0493(7) Uani 1 1 d . . . . .
C60 C 0.3355(2) 0.7092(2) 0.0986(2) 0.0491(6) Uani 1 1 d . . . . .
H60 H 0.3135 0.7270 0.0301 0.059 Uiso 1 1 calc R . . . .
C61 C 0.3457(2) 0.61485(19) 0.1251(2) 0.0431(6) Uani 1 1 d . . . . .
H61 H 0.3299 0.5685 0.0736 0.052 Uiso 1 1 calc R . . . .
C62 C 0.3518(3) 0.8825(2) 0.1457(3) 0.0686(10) Uani 1 1 d . . . . .
H62A H 0.3610 0.9210 0.2042 0.103 Uiso 1 1 calc GR . . . .
H62B H 0.2831 0.8965 0.0882 0.103 Uiso 1 1 calc GR . . . .
H62C H 0.4078 0.8977 0.1273 0.103 Uiso 1 1 calc GR . . . .


_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 Cl1 2.3197(7) . ?
Cr1 Cl2 2.3164(7) . ?
Cr1 O1 1.9799(18) . ?
Cr1 O1 2.0051(18) 2 ?
Cr1 N1 2.086(2) . ?
Cr1 N2 2.098(2) . ?
O1 Cr1 2.0051(18) 2 ?
O1 C6 1.418(3) . ?
N1 C1 1.346(3) . ?
N1 C5 1.349(3) . ?
N2 C7 1.333(4) . ?
N2 C11 1.341(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.382(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(4) . ?
C5 C6 1.506(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.391(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.387(4) . ?
C9 C10 1.388(4) . ?
C9 C12 1.507(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(4) . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
Cr51 Cl51 2.3272(7) . ?
Cr51 Cl52 2.3222(7) . ?
Cr51 O51 1.9865(18) . ?
Cr51 O51 1.9918(18) 2_655 ?
Cr51 N51 2.078(2) . ?
Cr51 N52 2.106(2) . ?
O51 Cr51 1.9919(18) 2_655 ?
O51 C56 1.425(3) . ?
N51 C51 1.346(3) . ?
N51 C55 1.350(3) . ?
N52 C57 1.337(3) . ?
N52 C61 1.346(3) . ?
C51 H51 0.9500 . ?
C51 C52 1.380(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.386(5) . ?
C53 H53 0.9500 . ?
C53 C54 1.381(4) . ?
C54 H54 0.9500 . ?
C54 C55 1.384(3) . ?
C55 C56 1.503(4) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57 0.9500 . ?
C57 C58 1.390(4) . ?
C58 H58 0.9500 . ?
C58 C59 1.379(5) . ?
C59 C60 1.390(4) . ?
C59 C62 1.505(4) . ?
C60 H60 0.9500 . ?
C60 C61 1.372(4) . ?
C61 H61 0.9500 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?

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
Cl2 Cr1 Cl1 93.53(3) . . ?
O1 Cr1 Cl1 94.66(6) . . ?
O1 Cr1 Cl1 171.59(6) 2 . ?
O1 Cr1 Cl2 94.37(6) 2 . ?
O1 Cr1 Cl2 168.90(5) . . ?
O1 Cr1 O1 77.90(8) . 2 ?
O1 Cr1 N1 79.45(7) . . ?
O1 Cr1 N1 96.95(7) 2 . ?
O1 Cr1 N2 95.99(7) . . ?
O1 Cr1 N2 85.66(7) 2 . ?
N1 Cr1 Cl1 85.40(6) . . ?
N1 Cr1 Cl2 93.77(6) . . ?
N1 Cr1 N2 174.10(9) . . ?
N2 Cr1 Cl1 91.28(6) . . ?
N2 Cr1 Cl2 91.30(6) . . ?
Cr1 O1 Cr1 102.10(8) . 2 ?
C6 O1 Cr1 119.81(16) . 2 ?
C6 O1 Cr1 112.12(14) . . ?
C1 N1 Cr1 128.66(19) . . ?
C1 N1 C5 118.5(2) . . ?
C5 N1 Cr1 112.55(16) . . ?
C7 N2 Cr1 119.79(17) . . ?
C7 N2 C11 117.7(2) . . ?
C11 N2 Cr1 122.49(19) . . ?
N1 C1 H1 119.0 . . ?
N1 C1 C2 122.1(3) . . ?
C2 C1 H1 119.0 . . ?
C1 C2 H2 120.2 . . ?
C1 C2 C3 119.6(2) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.6(3) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.1(3) . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 122.1(2) . . ?
N1 C5 C6 114.8(2) . . ?
C4 C5 C6 123.2(2) . . ?
O1 C6 C5 110.1(2) . . ?
O1 C6 H6A 109.6 . . ?
O1 C6 H6B 109.6 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 H7 118.6 . . ?
N2 C7 C8 122.8(3) . . ?
C8 C7 H7 118.6 . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.7(3) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 C10 116.9(2) . . ?
C8 C9 C12 120.9(3) . . ?
C10 C9 C12 122.2(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10 119.9 . . ?
N2 C11 C10 122.6(3) . . ?
N2 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Cl52 Cr51 Cl51 94.11(3) . . ?
O51 Cr51 Cl51 95.08(5) 2_655 . ?
O51 Cr51 Cl51 169.15(5) . . ?
O51 Cr51 Cl52 170.26(5) 2_655 . ?
O51 Cr51 Cl52 93.38(5) . . ?
O51 Cr51 O51 77.98(8) . 2_655 ?
O51 Cr51 N51 79.12(7) . . ?
O51 Cr51 N51 96.21(7) 2_655 . ?
O51 Cr51 N52 97.85(7) . . ?
O51 Cr51 N52 84.44(8) 2_655 . ?
N51 Cr51 Cl51 93.52(6) . . ?
N51 Cr51 Cl52 86.44(6) . . ?
N51 Cr51 N52 176.67(8) . . ?
N52 Cr51 Cl51 89.67(6) . . ?
N52 Cr51 Cl52 92.39(6) . . ?
Cr51 O51 Cr51 101.99(8) . 2_655 ?
C56 O51 Cr51 121.82(16) . 2_655 ?
C56 O51 Cr51 111.65(14) . . ?
C51 N51 Cr51 127.97(17) . . ?
C51 N51 C55 119.1(2) . . ?
C55 N51 Cr51 112.81(16) . . ?
C57 N52 Cr51 123.62(18) . . ?
C57 N52 C61 117.7(2) . . ?
C61 N52 Cr51 118.64(18) . . ?
N51 C51 H51 119.1 . . ?
N51 C51 C52 121.9(3) . . ?
C52 C51 H51 119.1 . . ?
C51 C52 H52 120.6 . . ?
C51 C52 C53 118.8(3) . . ?
C53 C52 H52 120.6 . . ?
C52 C53 H53 120.2 . . ?
C54 C53 C52 119.6(3) . . ?
C54 C53 H53 120.2 . . ?
C53 C54 H54 120.6 . . ?
C53 C54 C55 118.7(3) . . ?
C55 C54 H54 120.6 . . ?
N51 C55 C54 121.8(2) . . ?
N51 C55 C56 114.6(2) . . ?
C54 C55 C56 123.6(2) . . ?
O51 C56 C55 109.9(2) . . ?
O51 C56 H56A 109.7 . . ?
O51 C56 H56B 109.7 . . ?
C55 C56 H56A 109.7 . . ?
C55 C56 H56B 109.7 . . ?
H56A C56 H56B 108.2 . . ?
N52 C57 H57 119.0 . . ?
N52 C57 C58 121.9(3) . . ?
C58 C57 H57 119.0 . . ?
C57 C58 H58 119.7 . . ?
C59 C58 C57 120.5(3) . . ?
C59 C58 H58 119.7 . . ?
C58 C59 C60 116.9(3) . . ?
C58 C59 C62 122.3(3) . . ?
C60 C59 C62 120.7(3) . . ?
C59 C60 H60 120.1 . . ?
C61 C60 C59 119.9(3) . . ?
C61 C60 H60 120.1 . . ?
N52 C61 C60 123.0(3) . . ?
N52 C61 H61 118.5 . . ?
C60 C61 H61 118.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr1 O1 C6 C5 35.5(2) . . . . ?
Cr1 O1 C6 C5 -84.1(2) 2 . . . ?
Cr1 N1 C1 C2 -174.95(19) . . . . ?
Cr1 N1 C5 C4 176.6(2) . . . . ?
Cr1 N1 C5 C6 -3.3(3) . . . . ?
Cr1 N2 C7 C8 -179.6(2) . . . . ?
Cr1 N2 C11 C10 -179.6(2) . . . . ?
N1 C1 C2 C3 0.2(4) . . . . ?
N1 C5 C6 O1 -20.4(3) . . . . ?
N2 C7 C8 C9 -0.8(4) . . . . ?
C1 N1 C5 C4 1.8(4) . . . . ?
C1 N1 C5 C6 -178.1(2) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
C3 C4 C5 N1 -1.6(4) . . . . ?
C3 C4 C5 C6 178.3(2) . . . . ?
C4 C5 C6 O1 159.7(2) . . . . ?
C5 N1 C1 C2 -1.1(4) . . . . ?
C7 N2 C11 C10 0.7(4) . . . . ?
C7 C8 C9 C10 0.7(4) . . . . ?
C7 C8 C9 C12 179.5(3) . . . . ?
C8 C9 C10 C11 0.0(4) . . . . ?
C9 C10 C11 N2 -0.7(4) . . . . ?
C11 N2 C7 C8 0.1(4) . . . . ?
C12 C9 C10 C11 -178.8(3) . . . . ?
Cr51 O51 C56 C55 -84.4(2) 2_655 . . . ?
Cr51 O51 C56 C55 36.2(2) . . . . ?
Cr51 N51 C51 C52 -175.6(2) . . . . ?
Cr51 N51 C55 C54 175.0(2) . . . . ?
Cr51 N51 C55 C56 -5.4(3) . . . . ?
Cr51 N52 C57 C58 179.9(2) . . . . ?
Cr51 N52 C61 C60 -178.8(2) . . . . ?
N51 C51 C52 C53 1.3(4) . . . . ?
N51 C55 C56 O51 -19.5(3) . . . . ?
N52 C57 C58 C59 -2.0(4) . . . . ?
C51 N51 C55 C54 -1.7(4) . . . . ?
C51 N51 C55 C56 177.9(2) . . . . ?
C51 C52 C53 C54 -1.8(4) . . . . ?
C52 C53 C54 C55 0.7(4) . . . . ?
C53 C54 C55 N51 1.1(4) . . . . ?
C53 C54 C55 C56 -178.5(3) . . . . ?
C54 C55 C56 O51 160.1(2) . . . . ?
C55 N51 C51 C52 0.5(4) . . . . ?
C57 N52 C61 C60 0.4(4) . . . . ?
C57 C58 C59 C60 1.9(4) . . . . ?
C57 C58 C59 C62 -175.7(3) . . . . ?
C58 C59 C60 C61 -0.7(4) . . . . ?
C59 C60 C61 N52 -0.4(4) . . . . ?
C61 N52 C57 C58 0.8(4) . . . . ?
C62 C59 C60 C61 176.9(3) . . . . ?

_shelx_SHELXL_version_number     2014/7

_olex2_date_sample_data_collection 2016-08-05
_olex2_date_sample_submission    2016-08-05
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 679
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.655
_oxdiff_exptl_absorpt_empirical_full_min 0.770
