# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1579642'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
# local name eb16241

_audit_creation_date             2016-10-11
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H25 Cl2 Cr2 N2 O6, Cl'
_chemical_formula_sum            'C11 H25 Cl3 Cr2 N2 O6'
_chemical_formula_weight         491.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl'
_chemical_oxdiff_usercomment     '@ 120 K L1o'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.1130(3)
_cell_length_b                   10.2464(5)
_cell_length_c                   26.0466(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.273(4)
_cell_angle_gamma                90
_cell_volume                     1897.88(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5267
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.3980
_cell_measurement_theta_min      3.4820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.596
_exptl_absorpt_correction_T_max  0.96959
_exptl_absorpt_correction_T_min  0.96959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -6 33 0.0663
0 6 -33 0.0663
-10 0 -4 0.1801
10 2 -5 0.2143
1 -12 -20 0.0443
-1 12 20 0.0443
1 -14 7 0.0411
-1 14 -7 0.0411
8 0 22 0.1817
-5 -11 -11 0.1182
-1 14 10 0.0348
1 -14 -10 0.0348
-1 5 34 0.0588

_exptl_crystal_recrystallization_method 
'The material was recrystallised from acetonitrile by hydrothermal bomb'
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
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
-0.0052 -6.0060 32.9751 0.5267 -0.5362 0.6442
0.0052 6.0060 -32.9751 -0.5267 0.5362 -0.6442
-10.0018 -0.0201 -4.0094 0.3949 -0.3979 -0.8353
10.0029 2.0216 -4.9834 -0.5610 0.5344 0.6536
1.0176 -11.9899 -20.0008 0.6042 0.7904 -0.0566
-1.0176 11.9899 20.0008 -0.6042 -0.7904 0.0566
1.0107 -13.9956 6.9820 0.8557 0.2741 0.4227
-1.0107 13.9956 -6.9820 -0.8557 -0.2741 -0.4227
7.9954 0.0117 21.9970 -0.2268 -0.0783 0.9791
-4.9880 -11.0048 -11.0116 0.8335 0.2845 -0.3857
-1.0162 13.9916 10.0085 -0.7750 -0.6328 -0.1416
1.0162 -13.9916 -10.0085 0.7750 0.6328 0.1416
-1.0158 4.9886 33.9853 -0.1059 -0.8990 0.4031

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            111506
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.753
_diffrn_reflns_theta_min         3.076
_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 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  83.00   1.00   10.00    --  -19.68  77.00-150.00  147
  2  ω    -20.00  73.00   1.00   10.00    --   21.16 -99.00-180.00   93
  3  ω    -20.00  73.00   1.00   10.00    --   21.16 -99.00  60.00   93
  4  ω    -22.00 115.00   1.00   10.00    --   21.16  57.00 120.00  137
  5  ω    -23.00 124.00   1.00   10.00    --   21.16  77.00 -90.00  147
  6  ω    -22.00 115.00   1.00   10.00    --   21.16  57.00  30.00  137
  7  ω    -20.00  11.00   1.00   10.00    --  -19.68 -99.00 120.00   31
  8  ω    -63.00  74.00   1.00   10.00    --  -19.68  57.00   0.00  137
;
_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      -0.0412507000
_diffrn_orient_matrix_UB_12      -0.0617633000
_diffrn_orient_matrix_UB_13      0.0047166000
_diffrn_orient_matrix_UB_21      0.0482949000
_diffrn_orient_matrix_UB_22      -0.0266254000
_diffrn_orient_matrix_UB_23      -0.0211017000
_diffrn_orient_matrix_UB_31      0.0769077000
_diffrn_orient_matrix_UB_32      -0.0163827000
_diffrn_orient_matrix_UB_33      0.0165655000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5411
_reflns_number_total             5954
_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 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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         0.552
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.118
_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)+(0.0369P)²+3.9375P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0984
_refine_special_details          
;
The diffraction pattern was affected by non-merohedral twinning.  This was handled using CrysAlisPro and twin law [1 0 0 / 0 -1 0 / -0.1593 0 -1] and twin scale factor 0.5201(14).  O-bound H atoms were identified from a difference Fourier map and refined freely.


 
#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          4 Note
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
432_ALERT_2_G Short Inter X...Y Contact  O5     ..  C11     ..       3.00 Ang.
793_ALERT_4_G The Model has Chirality at N1      (Centro SPGR)          S Verify
793_ALERT_4_G The Model has Chirality at N2      (Centro SPGR)          S Verify
860_ALERT_3_G Number of Least-Squares Restraints .............          2 Note
870_ALERT_4_G ALERTS Related to Twinning Effects Suppressed ..          ! Info
952_ALERT_5_G Calculated (ThMax) and CIF-Reported Lmax Differ           2 Units

None of the above are significant.

#===============================================================================
 
#===============================================================================
! Congratulations ! : No (A,B,C) ALERT Conditions were Detected - Check G-ALERTS
#===============================================================================
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4795(10) 0.5205(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O2-H2 = O4-H4
 0.84 with sigma of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.87590(8) 0.52412(6) 0.62079(2) 0.01065(14) Uani 1 1 d . . . . .
Cr2 Cr 0.89044(8) 0.23509(6) 0.61510(2) 0.01074(14) Uani 1 1 d . . . . .
Cl1 Cl 0.71547(14) 0.68825(9) 0.57705(4) 0.0178(2) Uani 1 1 d . . . . .
Cl2 Cl 1.10025(14) 0.06851(9) 0.63156(4) 0.0201(2) Uani 1 1 d . . . . .
O1 O 1.0028(3) 0.3774(3) 0.65540(11) 0.0130(6) Uani 1 1 d . . . . .
O2 O 0.7264(4) 0.5643(3) 0.68306(11) 0.0151(6) Uani 1 1 d D . . . .
H2 H 0.686(6) 0.502(3) 0.6990(16) 0.018 Uiso 1 1 d DR . . . .
O3 O 0.7127(3) 0.3781(2) 0.59970(10) 0.0108(5) Uani 1 1 d . . . . .
O4 O 0.7378(4) 0.1700(3) 0.67332(11) 0.0160(6) Uani 1 1 d D . . . .
H4 H 0.702(6) 0.215(4) 0.6968(14) 0.019 Uiso 1 1 d DR . . . .
O5 O 1.0424(4) 0.4999(3) 0.56117(11) 0.0139(6) Uani 1 1 d . . . . .
O6 O 1.0387(4) 0.2809(3) 0.55442(11) 0.0157(6) Uani 1 1 d . . . . .
N1 N 1.0775(4) 0.6364(3) 0.66025(13) 0.0139(7) Uani 1 1 d . . . . .
N2 N 0.6924(4) 0.1268(3) 0.57174(14) 0.0146(7) Uani 1 1 d . . . . .
C1 C 1.1923(6) 0.5440(4) 0.69288(17) 0.0171(9) Uani 1 1 d . . . . .
H1A H 1.1388 0.5376 0.7267 0.021 Uiso 1 1 calc R . . . .
H1B H 1.3198 0.5766 0.6968 0.021 Uiso 1 1 calc R . . . .
C2 C 1.1947(5) 0.4091(4) 0.66766(17) 0.0146(8) Uani 1 1 d . . . . .
H2A H 1.2684 0.4110 0.6368 0.018 Uiso 1 1 calc R . . . .
H2B H 1.2489 0.3450 0.6911 0.018 Uiso 1 1 calc R . . . .
C3 C 0.9660(6) 0.7267(4) 0.69273(17) 0.0187(9) Uani 1 1 d . . . . .
H3A H 0.9095 0.7941 0.6713 0.022 Uiso 1 1 calc R . . . .
H3B H 1.0487 0.7685 0.7178 0.022 Uiso 1 1 calc R . . . .
C4 C 0.8138(6) 0.6533(4) 0.72003(16) 0.0189(9) Uani 1 1 d . . . . .
H4A H 0.8674 0.6049 0.7488 0.023 Uiso 1 1 calc R . . . .
H4B H 0.7211 0.7138 0.7329 0.023 Uiso 1 1 calc R . . . .
C5 C 1.2030(6) 0.7135(4) 0.62683(18) 0.0232(10) Uani 1 1 d . . . . .
H5A H 1.1282 0.7626 0.6025 0.035 Uiso 1 1 calc GR . . . .
H5B H 1.2842 0.6554 0.6088 0.035 Uiso 1 1 calc GR . . . .
H5C H 1.2774 0.7721 0.6476 0.035 Uiso 1 1 calc GR . . . .
C6 C 0.5402(5) 0.2199(4) 0.55357(17) 0.0182(9) Uani 1 1 d . . . . .
H6A H 0.4955 0.1947 0.5195 0.022 Uiso 1 1 calc R . . . .
H6B H 0.4350 0.2158 0.5766 0.022 Uiso 1 1 calc R . . . .
C7 C 0.6151(6) 0.3568(4) 0.55211(15) 0.0157(8) Uani 1 1 d . . . . .
H7A H 0.6998 0.3671 0.5237 0.019 Uiso 1 1 calc R . . . .
H7B H 0.5128 0.4187 0.5479 0.019 Uiso 1 1 calc R . . . .
C8 C 0.6173(6) 0.0284(4) 0.60815(17) 0.0201(9) Uani 1 1 d . . . . .
H8A H 0.7088 -0.0407 0.6136 0.024 Uiso 1 1 calc R . . . .
H8B H 0.5033 -0.0102 0.5937 0.024 Uiso 1 1 calc R . . . .
C9 C 0.5755(6) 0.0928(4) 0.65865(18) 0.0215(9) Uani 1 1 d . . . . .
H9A H 0.4653 0.1481 0.6550 0.026 Uiso 1 1 calc R . . . .
H9B H 0.5516 0.0274 0.6846 0.026 Uiso 1 1 calc R . . . .
C10 C 0.7747(6) 0.0592(4) 0.52686(18) 0.0223(10) Uani 1 1 d . . . . .
H10A H 0.8801 0.0074 0.5382 0.033 Uiso 1 1 calc GR . . . .
H10B H 0.8156 0.1228 0.5025 0.033 Uiso 1 1 calc GR . . . .
H10C H 0.6815 0.0038 0.5110 0.033 Uiso 1 1 calc GR . . . .
C11 C 1.0871(5) 0.3932(4) 0.54098(15) 0.0146(8) Uani 1 1 d . . . . .
H11 H 1.1650 0.3981 0.5128 0.017 Uiso 1 1 calc R . . . .
Cl3 Cl 0.59157(14) 0.35388(10) 0.74917(4) 0.0191(2) 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 2.3175(11) . ?
Cr1 O1 1.963(3) . ?
Cr1 O2 2.002(3) . ?
Cr1 O3 1.964(3) . ?
Cr1 O5 1.989(3) . ?
Cr1 N1 2.091(3) . ?
Cr2 Cl2 2.3012(11) . ?
Cr2 O1 1.957(3) . ?
Cr2 O3 1.971(3) . ?
Cr2 O4 1.999(3) . ?
Cr2 O6 1.976(3) . ?
Cr2 N2 2.103(3) . ?
O1 C2 1.433(4) . ?
O2 H2 0.81(2) . ?
O2 C4 1.456(5) . ?
O3 C7 1.424(4) . ?
O4 H4 0.81(2) . ?
O4 C9 1.444(5) . ?
O5 C11 1.258(5) . ?
O6 C11 1.253(5) . ?
N1 C1 1.502(5) . ?
N1 C3 1.493(5) . ?
N1 C5 1.487(5) . ?
N2 C6 1.511(5) . ?
N2 C8 1.491(5) . ?
N2 C10 1.490(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.530(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.509(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.501(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.507(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11 0.9300 . ?

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 176.51(9) . . ?
O1 Cr1 O2 91.87(12) . . ?
O1 Cr1 O3 78.91(11) . . ?
O1 Cr1 O5 89.29(12) . . ?
O1 Cr1 N1 83.84(12) . . ?
O2 Cr1 Cl1 89.10(9) . . ?
O2 Cr1 N1 81.93(12) . . ?
O3 Cr1 Cl1 97.69(8) . . ?
O3 Cr1 O2 93.55(11) . . ?
O3 Cr1 O5 92.58(11) . . ?
O3 Cr1 N1 162.02(12) . . ?
O5 Cr1 Cl1 90.10(9) . . ?
O5 Cr1 O2 173.87(12) . . ?
O5 Cr1 N1 92.21(12) . . ?
N1 Cr1 Cl1 99.62(9) . . ?
O1 Cr2 Cl2 101.38(8) . . ?
O1 Cr2 O3 78.90(11) . . ?
O1 Cr2 O4 93.65(12) . . ?
O1 Cr2 O6 91.91(12) . . ?
O1 Cr2 N2 160.42(12) . . ?
O3 Cr2 Cl2 178.92(9) . . ?
O3 Cr2 O4 92.62(11) . . ?
O3 Cr2 O6 90.68(11) . . ?
O3 Cr2 N2 82.20(11) . . ?
O4 Cr2 Cl2 88.40(9) . . ?
O4 Cr2 N2 82.11(13) . . ?
O6 Cr2 Cl2 88.27(9) . . ?
O6 Cr2 O4 173.99(12) . . ?
O6 Cr2 N2 93.37(13) . . ?
N2 Cr2 Cl2 97.62(9) . . ?
Cr2 O1 Cr1 98.42(12) . . ?
C2 O1 Cr1 110.8(2) . . ?
C2 O1 Cr2 131.7(2) . . ?
Cr1 O2 H2 117(3) . . ?
C4 O2 Cr1 116.0(2) . . ?
C4 O2 H2 107(3) . . ?
Cr1 O3 Cr2 97.88(11) . . ?
C7 O3 Cr1 129.3(2) . . ?
C7 O3 Cr2 111.2(2) . . ?
Cr2 O4 H4 124(3) . . ?
C9 O4 Cr2 115.2(3) . . ?
C9 O4 H4 104(3) . . ?
C11 O5 Cr1 126.5(3) . . ?
C11 O6 Cr2 126.6(3) . . ?
C1 N1 Cr1 106.8(2) . . ?
C3 N1 Cr1 104.6(2) . . ?
C3 N1 C1 111.0(3) . . ?
C5 N1 Cr1 114.7(3) . . ?
C5 N1 C1 109.9(3) . . ?
C5 N1 C3 109.6(3) . . ?
C6 N2 Cr2 107.5(2) . . ?
C8 N2 Cr2 105.1(3) . . ?
C8 N2 C6 111.2(3) . . ?
C10 N2 Cr2 113.4(2) . . ?
C10 N2 C6 109.8(3) . . ?
C10 N2 C8 109.7(3) . . ?
N1 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
N1 C1 C2 109.7(3) . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
O1 C2 C1 106.3(3) . . ?
O1 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 C4 110.8(3) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
O2 C4 C3 107.5(3) . . ?
O2 C4 H4A 110.2 . . ?
O2 C4 H4B 110.2 . . ?
C3 C4 H4A 110.2 . . ?
C3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.6 . . ?
N2 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 N2 110.2(3) . . ?
C7 C6 H6A 109.6 . . ?
C7 C6 H6B 109.6 . . ?
O3 C7 C6 106.7(3) . . ?
O3 C7 H7A 110.4 . . ?
O3 C7 H7B 110.4 . . ?
C6 C7 H7A 110.4 . . ?
C6 C7 H7B 110.4 . . ?
H7A C7 H7B 108.6 . . ?
N2 C8 H8A 109.7 . . ?
N2 C8 H8B 109.7 . . ?
N2 C8 C9 109.8(3) . . ?
H8A C8 H8B 108.2 . . ?
C9 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
O4 C9 C8 107.4(3) . . ?
O4 C9 H9A 110.2 . . ?
O4 C9 H9B 110.2 . . ?
C8 C9 H9A 110.2 . . ?
C8 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 H11 116.3 . . ?
O6 C11 O5 127.5(4) . . ?
O6 C11 H11 116.3 . . ?

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 C2 C1 47.7(4) . . . . ?
Cr1 O2 C4 C3 19.0(4) . . . . ?
Cr1 O3 C7 C6 170.2(2) . . . . ?
Cr1 O5 C11 O6 -1.0(6) . . . . ?
Cr1 N1 C1 C2 28.5(4) . . . . ?
Cr1 N1 C3 C4 46.5(4) . . . . ?
Cr2 O1 C2 C1 170.9(3) . . . . ?
Cr2 O3 C7 C6 49.7(3) . . . . ?
Cr2 O4 C9 C8 27.7(4) . . . . ?
Cr2 O6 C11 O5 -4.8(6) . . . . ?
Cr2 N2 C6 C7 23.9(4) . . . . ?
Cr2 N2 C8 C9 44.7(3) . . . . ?
N1 C1 C2 O1 -49.9(4) . . . . ?
N1 C3 C4 O2 -43.7(4) . . . . ?
N2 C6 C7 O3 -47.5(4) . . . . ?
N2 C8 C9 O4 -48.1(4) . . . . ?
C1 N1 C3 C4 -68.4(4) . . . . ?
C3 N1 C1 C2 142.0(3) . . . . ?
C5 N1 C1 C2 -96.5(4) . . . . ?
C5 N1 C3 C4 170.0(3) . . . . ?
C6 N2 C8 C9 -71.4(4) . . . . ?
C8 N2 C6 C7 138.5(4) . . . . ?
C10 N2 C6 C7 -99.9(4) . . . . ?
C10 N2 C8 C9 166.9(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_submission    2016-10-10
_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 L1o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.532
_oxdiff_exptl_absorpt_empirical_full_min 0.620
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4795(10) 1993 30210 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.5205(10) 2051 30210 nmt 0.9999 0.0002 0.0000 -0.0000 -0.9998 -0.0001
-0.1593 -0.0007 -1.0002

_twin_special_details            
;
Component 2 rotated by -179.9847° 
 around [1.00 -0.00 -0.08] (reciprocal) or [1.00 0.00 0.00] (direct)
;
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1579650'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT770_9                   
;
PROBLEM: Suspect C-H Bond in CIF:   C22    --  H20A    ..       1.39 Ang.
RESPONSE: Please see the _refine_special_details section of the CIF.
;
# Added during the CSD deposition process: Thursday 12 October 2017 12:17 PM
# end Validation Reply Form


# local name eb17025


_audit_creation_date             2017-02-15
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C19 H33 Cl2 Cr2 N2 O6), 2(Cl), C4 H10 O'
_chemical_formula_sum            'C42 H76 Cl6 Cr4 N4 O13'
_chemical_formula_weight         1265.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl'
_chemical_oxdiff_usercomment     '@ 120 K 449o'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.1699(2)
_cell_length_b                   11.0066(3)
_cell_length_c                   34.9817(7)
_cell_angle_alpha                90
_cell_angle_beta                 93.103(2)
_cell_angle_gamma                90
_cell_volume                     2756.58(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    19210
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.2500
_cell_measurement_theta_min      3.3920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0782 before and 0.0619 after correction. The Ratio of minimum to maximum transmission is 0.8566. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0462
0 0 1 0.0462
-5 -2 -4 0.1602
0 5 1 0.0116
0 -5 -1 0.0350
5 1 2 0.1578

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of diethyl ether and acetonitrile by vapour diffusion'
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.047
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
0.0000 0.0002 -0.9987 0.0056 -0.0194 -0.0020
-0.0000 -0.0002 0.9987 -0.0056 0.0194 0.0020
-4.9954 -1.9937 -4.0021 0.0773 -0.1423 0.4961
0.0013 4.9928 1.0018 -0.3111 -0.0626 -0.0573
-0.0013 -4.9928 -1.0018 0.3111 0.0626 0.0573
4.9951 0.9955 2.0041 -0.0050 0.1199 -0.4883

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            48300
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.773
_diffrn_reflns_theta_min         2.845
_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 0.999
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  30.00   1.00   10.00    --   -9.43 -99.00  60.00   50
  2  ω    -12.00  83.00   1.00   10.00    --   10.84  38.00 -30.00   95
  3  ω    -26.00  89.00   1.00   10.00    --   10.84  19.00-180.00  115
  4  ω    -12.00  83.00   1.00   10.00    --   10.84  38.00-180.00   95
  5  ω      1.00  79.00   1.00   10.00    --   10.84  38.00-120.00   78
  6  ω    -36.00  26.00   1.00   10.00    --   10.84 -38.00  30.00   62
  7  ω     -8.00  35.00   1.00   10.00    --   10.84 -57.00-120.00   43
  8  ω      1.00  79.00   1.00   10.00    --   10.84  77.00 -30.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       ?
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0134360000
_diffrn_orient_matrix_UB_12      -0.0611892000
_diffrn_orient_matrix_UB_13      -0.0056029000
_diffrn_orient_matrix_UB_21      0.0194878000
_diffrn_orient_matrix_UB_22      -0.0164330000
_diffrn_orient_matrix_UB_23      0.0194097000
_diffrn_orient_matrix_UB_31      -0.0961969000
_diffrn_orient_matrix_UB_32      -0.0118539000
_diffrn_orient_matrix_UB_33      0.0020192000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) 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                5556
_reflns_number_total             7202
_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 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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         0.449
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7202
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0407
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0269P)²+2.7526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0860
_refine_special_details          
;
The diethyl ether molecule has been modelled as disordered about a crystallographic inversion centre.  Appropriate adjustments were made to site occupancy factors such that the total sums to 0.5 Et2O per asymmetric unit.  H atoms for the methylene C atom could not be placed using an HFIX instruction and so were identified from a difference Fourier map and refined as half-occupied with appropriate geometric restraints.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
770_ALERT_2_A Suspect C-H Bond in CIF:   C22    --  H20A    ..       1.39 Ang.

Consequence of diethyl ether disorder.

#===============================================================================
420_ALERT_2_B D-H Without Acceptor      *O7     -- *H20B   ...     Please Check
420_ALERT_2_B D-H Without Acceptor      *O7     -- *H20C   ...     Please Check
772_ALERT_2_B Suspect O-H Bond in CIF:   O7     --  H20C    ..       1.41 Ang.

Consequence of diethyl ether disorder.


#===============================================================================
772_ALERT_2_C Suspect O-H Bond in CIF:   O7     --  H20B    ..       1.39 Ang.

Consequence of diethyl ether disorder.

906_ALERT_3_C Large K value in the Analysis of Variance ......      7.150 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           5 Note
977_ALERT_2_C Check the Negative Difference Density on    H22C      -0.31 eA-3

Noted

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         12 Note
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          2 Report
173_ALERT_4_G The CIF-Embedded .res File Contains DANG Records          2 Report
176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          1 Report
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr2    --  Cl2     ..        5.7 s.u.
300_ALERT_4_G Atom Site Occupancy of *O7     is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *C21    is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *C22    is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H20A   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H20B   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H20C   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H20D   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H21A   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H21B   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H21C   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H22A   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H22B   is Constrained at        0.5 Check
300_ALERT_4_G Atom Site Occupancy of *H22C   is Constrained at        0.5 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1)..          6 % Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2)..         60 % Note
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        167 Check
              C20  -O7   -H20B    1.555   1.555   1.555             41.70 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        168 Check
              C20  -O7   -H20C    1.555   1.555   1.555             41.00 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        202 Check
              C20  -C21  -H20C    1.555   1.555   1.555             37.90 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        212 Check
              C20  -C22  -H20A    1.555   1.555   1.555             40.20 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        213 Check
              C20  -C22  -H20D    1.555   1.555   1.555             42.40 Deg.
793_ALERT_4_G The Model has Chirality at N1      (Centro SPGR)          S Verify
860_ALERT_3_G Number of Least-Squares Restraints .............          9 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        651 Note
978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          5 Note

There is nothing serious here - most of these Alerts are a consequence of diethyl ether disorder.

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H19,H2,H4} of C19, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  {H12A,H12B,H12C} of C12, {H12D,H12E,H12F} of C12A, {H21A,H21B,H21C} of C21,
  {H22A,H22B,H22C} of C22, {H6A,H6B,H6C} of C6
2. Restrained distances
 C20-H20B = C20-H20A = C20-H20D = C20-H20C
 0.97 with sigma of 0.02
 O2-H2 = O4-H4
 0.84 with sigma of 0.02
 H20D-H20A
 1.564 with sigma of 0.04
 H20C-H20B
 1.564 with sigma of 0.04
 N2-C11A \\sim N2-C11
 with sigma of 0.02
3. Others
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: O7(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) H20A(0.5) H20B(0.5) H20C(0.5) H20D(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C11A(H11C,H11D)
4.b Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
4.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.36988(4) 0.28419(3) 0.65512(2) 0.01284(9) Uani 1 1 d . . . . .
Cr2 Cr 0.35170(5) 0.55365(3) 0.65181(2) 0.01605(9) Uani 1 1 d . . . . .
Cl1 Cl 0.58881(7) 0.13605(5) 0.66934(2) 0.01962(12) Uani 1 1 d . . . . .
Cl2 Cl 0.17935(8) 0.69277(6) 0.61558(2) 0.02636(14) Uani 1 1 d . . . . .
O1 O 0.18756(19) 0.41337(15) 0.64239(4) 0.0166(3) Uani 1 1 d . . . . .
O2 O 0.2416(2) 0.23678(15) 0.70207(4) 0.0174(3) Uani 1 1 d D . . . .
O3 O 0.48677(19) 0.42543(14) 0.68038(4) 0.0150(3) Uani 1 1 d . . . . .
O4 O 0.2190(2) 0.60650(16) 0.69802(5) 0.0230(4) Uani 1 1 d D . . . .
O5 O 0.4981(2) 0.51822(15) 0.60668(4) 0.0205(3) Uani 1 1 d . . . . .
O6 O 0.4902(2) 0.31472(14) 0.60667(4) 0.0160(3) Uani 1 1 d . . . . .
N1 N 0.1621(2) 0.17267(18) 0.62826(5) 0.0171(4) Uani 1 1 d . . . . .
N2 N 0.5607(2) 0.66589(18) 0.67750(5) 0.0175(4) Uani 1 1 d D . . . .
C1 C 0.0024(3) 0.2549(2) 0.61547(7) 0.0228(5) Uani 1 1 d . . . . .
H1A H -0.091935 0.255682 0.635115 0.027 Uiso 1 1 calc R . . . .
H1B H -0.058058 0.223777 0.591314 0.027 Uiso 1 1 calc R . . . .
C2 C 0.0726(3) 0.3824(2) 0.60940(6) 0.0202(5) Uani 1 1 d . . . . .
H2A H 0.145502 0.385944 0.586182 0.024 Uiso 1 1 calc R . . . .
H2B H -0.033579 0.439622 0.606182 0.024 Uiso 1 1 calc R . . . .
C3 C 0.1053(3) 0.0890(2) 0.65910(6) 0.0218(5) Uani 1 1 d . . . . .
H3A H 0.201894 0.025625 0.663655 0.026 Uiso 1 1 calc R . . . .
H3B H -0.013494 0.048412 0.650977 0.026 Uiso 1 1 calc R . . . .
C4 C 0.0809(3) 0.1588(2) 0.69549(7) 0.0267(6) Uani 1 1 d . . . . .
H4A H -0.034565 0.208089 0.693112 0.032 Uiso 1 1 calc R . . . .
H4B H 0.070939 0.101909 0.717212 0.032 Uiso 1 1 calc R . . . .
C5 C 0.2320(3) 0.1031(2) 0.59512(7) 0.0250(5) Uani 1 1 d . . . . .
H5A H 0.350998 0.063203 0.603509 0.030 Uiso 1 1 calc R . . . .
H5B H 0.259483 0.161501 0.574640 0.030 Uiso 1 1 calc R . . . .
C6 C 0.0993(4) 0.0069(3) 0.57830(8) 0.0330(6) Uani 1 1 d . . . . .
H6A H 0.080777 -0.056140 0.597497 0.049 Uiso 1 1 calc GR . . . .
H6B H 0.152688 -0.029590 0.555793 0.049 Uiso 1 1 calc GR . . . .
H6C H -0.021001 0.044526 0.570760 0.049 Uiso 1 1 calc GR . . . .
C7 C 0.6740(3) 0.5856(2) 0.70459(7) 0.0240(5) Uani 1 1 d . . . . .
H7A H 0.803240 0.617107 0.707800 0.029 Uiso 1 1 calc R . . . .
H7B H 0.619201 0.585846 0.729957 0.029 Uiso 1 1 calc R . . . .
C8 C 0.6771(3) 0.4581(2) 0.68930(7) 0.0202(5) Uani 1 1 d . . . . .
H8A H 0.749903 0.454347 0.666074 0.024 Uiso 1 1 calc R . . . .
H8B H 0.734467 0.402185 0.708740 0.024 Uiso 1 1 calc R . . . .
C9 C 0.4569(3) 0.7603(2) 0.69845(7) 0.0250(5) Uani 1 1 d . . . . .
H9A H 0.397992 0.818588 0.679921 0.030 Uiso 1 1 calc R . . . .
H9B H 0.545046 0.805801 0.715882 0.030 Uiso 1 1 calc R . . . .
C10 C 0.3078(3) 0.7013(3) 0.72137(7) 0.0283(6) Uani 1 1 d . . . . .
H10A H 0.364865 0.666089 0.745284 0.034 Uiso 1 1 calc R . . . .
H10B H 0.214146 0.762498 0.728242 0.034 Uiso 1 1 calc R . . . .
C11 C 0.6685(19) 0.7200(16) 0.6461(3) 0.023(2) Uani 0.503(7) 1 d D . P A 1
H11A H 0.579868 0.751900 0.625811 0.027 Uiso 0.503(7) 1 calc R . P A 1
H11B H 0.744086 0.655670 0.634563 0.027 Uiso 0.503(7) 1 calc R . P A 1
C11A C 0.7083(19) 0.7293(16) 0.6544(3) 0.028(3) Uani 0.497(7) 1 d D . P A 2
H11C H 0.786275 0.779956 0.672411 0.033 Uiso 0.497(7) 1 calc R . P A 2
H11D H 0.790532 0.665799 0.644487 0.033 Uiso 0.497(7) 1 calc R . P A 2
C12 C 0.7953(7) 0.8209(5) 0.66039(14) 0.0239(13) Uani 0.503(7) 1 d . . P A 1
H12A H 0.720177 0.887313 0.670155 0.036 Uiso 0.503(7) 1 calc GR . P A 1
H12B H 0.867570 0.850931 0.639358 0.036 Uiso 0.503(7) 1 calc GR . P A 1
H12C H 0.880680 0.790301 0.680998 0.036 Uiso 0.503(7) 1 calc GR . P A 1
C12A C 0.6424(8) 0.8089(5) 0.62113(15) 0.0317(15) Uani 0.497(7) 1 d . . P A 2
H12D H 0.547098 0.765628 0.605275 0.048 Uiso 0.497(7) 1 calc GR . P A 2
H12E H 0.748354 0.828636 0.605695 0.048 Uiso 0.497(7) 1 calc GR . P A 2
H12F H 0.588975 0.884088 0.630843 0.048 Uiso 0.497(7) 1 calc GR . P A 2
C13 C 0.5319(3) 0.4160(2) 0.59236(6) 0.0153(4) Uani 1 1 d . . . . .
C14 C 0.6252(3) 0.4136(2) 0.55526(6) 0.0158(4) Uani 1 1 d . . . . .
C15 C 0.6797(3) 0.5212(2) 0.53851(7) 0.0223(5) Uani 1 1 d . . . . .
H15 H 0.662312 0.596585 0.551055 0.027 Uiso 1 1 calc R . . . .
C16 C 0.7598(3) 0.5180(3) 0.50329(7) 0.0331(7) Uani 1 1 d . . . . .
H16 H 0.796936 0.591560 0.491704 0.040 Uiso 1 1 calc R . . . .
C17 C 0.7858(3) 0.4091(3) 0.48503(7) 0.0339(7) Uani 1 1 d . . . . .
H17 H 0.839583 0.407848 0.460801 0.041 Uiso 1 1 calc R . . . .
C18 C 0.7340(3) 0.3018(3) 0.50176(7) 0.0278(6) Uani 1 1 d . . . . .
H18 H 0.753556 0.226777 0.489183 0.033 Uiso 1 1 calc R . . . .
C19 C 0.6533(3) 0.3031(2) 0.53697(6) 0.0188(5) Uani 1 1 d . . . . .
H19 H 0.617495 0.229188 0.548506 0.023 Uiso 1 1 calc R . . . .
H2 H 0.212(4) 0.293(2) 0.7157(7) 0.023 Uiso 1 1 d DR . . . .
H4 H 0.178(4) 0.553(2) 0.7113(7) 0.023 Uiso 1 1 d DR . . . .
Cl3 Cl 0.09381(8) 0.42012(7) 0.75153(2) 0.03325(16) Uani 1 1 d . . . . .
O7 O 0.4380(5) 0.0172(4) 0.51728(10) 0.0328(9) Uani 0.5 1 d . . P . .
C20 C 0.3885(4) 0.0586(3) 0.48139(8) 0.0354(7) Uani 1 1 d D . . . .
C21 C 0.2199(8) 0.1482(5) 0.48566(15) 0.0331(12) Uani 0.5 1 d . . P . .
H21A H 0.179328 0.180420 0.460448 0.050 Uiso 0.5 1 calc R . P . .
H21B H 0.116136 0.104576 0.496573 0.050 Uiso 0.5 1 calc R . P . .
H21C H 0.259180 0.215400 0.502621 0.050 Uiso 0.5 1 calc R . P . .
C22 C 0.3654(8) 0.1097(6) 0.44309(17) 0.0383(14) Uani 0.5 1 d . . P . .
H22A H 0.237594 0.095118 0.432773 0.057 Uiso 0.5 1 calc R . P . .
H22B H 0.389168 0.197385 0.444210 0.057 Uiso 0.5 1 calc R . P . .
H22C H 0.453949 0.071168 0.426491 0.057 Uiso 0.5 1 calc R . P . .
H20A H 0.351(8) -0.001(4) 0.4617(13) 0.046 Uiso 0.5 1 d DR . P . .
H20B H 0.305(7) -0.007(4) 0.4881(17) 0.046 Uiso 0.5 1 d DR . P . .
H20C H 0.360(8) 0.122(4) 0.4996(14) 0.046 Uiso 0.5 1 d DR . P . .
H20D H 0.477(7) 0.109(5) 0.4677(15) 0.046 Uiso 0.5 1 d DR . P . .


_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 2.2990(6) . ?
Cr1 O1 1.9662(15) . ?
Cr1 O2 1.9946(15) . ?
Cr1 O3 1.9543(15) . ?
Cr1 O6 1.9721(14) . ?
Cr1 N1 2.1113(19) . ?
Cr2 Cl2 2.3041(7) . ?
Cr2 O1 1.9585(16) . ?
Cr2 O3 1.9553(15) . ?
Cr2 O4 2.0057(16) . ?
Cr2 O5 1.9815(16) . ?
Cr2 N2 2.1054(19) . ?
O1 C2 1.423(2) . ?
O2 C4 1.445(3) . ?
O2 H2 0.817(17) . ?
O3 C8 1.429(3) . ?
O4 C10 1.451(3) . ?
O4 H4 0.817(17) . ?
O5 C13 1.261(3) . ?
O6 C13 1.264(3) . ?
N1 C1 1.508(3) . ?
N1 C3 1.492(3) . ?
N1 C5 1.498(3) . ?
N2 C7 1.502(3) . ?
N2 C9 1.494(3) . ?
N2 C11 1.501(10) . ?
N2 C11A 1.533(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.509(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.505(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.521(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.502(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.517(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.504(12) . ?
C11A H11C 0.9900 . ?
C11A H11D 0.9900 . ?
C11A C12A 1.513(15) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C13 C14 1.492(3) . ?
C14 C15 1.387(3) . ?
C14 C19 1.394(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.376(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.377(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.389(3) . ?
C19 H19 0.9500 . ?
O7 C20 1.497(5) 3_656 ?
O7 C20 1.365(4) . ?
O7 H20B 1.39(6) . ?
O7 H20C 1.41(6) . ?
C20 C21 1.573(7) . ?
C20 C22 1.454(6) . ?
C20 H20A 0.981(19) . ?
C20 H20B 0.980(19) . ?
C20 H20C 0.973(19) . ?
C20 H20D 0.984(19) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 H20C 1.13(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 H20A 1.39(6) . ?
C22 H20D 1.14(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 Cl1 178.55(5) . . ?
O1 Cr1 O2 92.59(7) . . ?
O1 Cr1 O6 89.92(6) . . ?
O1 Cr1 N1 82.83(7) . . ?
O2 Cr1 Cl1 88.64(5) . . ?
O2 Cr1 N1 82.46(7) . . ?
O3 Cr1 Cl1 101.26(5) . . ?
O3 Cr1 O1 77.92(6) . . ?
O3 Cr1 O2 92.38(6) . . ?
O3 Cr1 O6 93.22(6) . . ?
O3 Cr1 N1 159.83(7) . . ?
O6 Cr1 Cl1 88.93(5) . . ?
O6 Cr1 O2 174.24(7) . . ?
O6 Cr1 N1 92.72(7) . . ?
N1 Cr1 Cl1 98.10(6) . . ?
O1 Cr2 Cl2 97.58(5) . . ?
O1 Cr2 O4 93.28(7) . . ?
O1 Cr2 O5 92.88(7) . . ?
O1 Cr2 N2 160.34(7) . . ?
O3 Cr2 Cl2 175.45(5) . . ?
O3 Cr2 O1 78.08(6) . . ?
O3 Cr2 O4 92.35(7) . . ?
O3 Cr2 O5 89.78(6) . . ?
O3 Cr2 N2 83.34(7) . . ?
O4 Cr2 Cl2 89.24(5) . . ?
O4 Cr2 N2 81.01(7) . . ?
O5 Cr2 Cl2 89.08(5) . . ?
O5 Cr2 O4 173.79(7) . . ?
O5 Cr2 N2 93.44(7) . . ?
N2 Cr2 Cl2 101.13(6) . . ?
Cr2 O1 Cr1 98.39(6) . . ?
C2 O1 Cr1 111.04(13) . . ?
C2 O1 Cr2 129.93(14) . . ?
Cr1 O2 H2 115.2(19) . . ?
C4 O2 Cr1 115.05(13) . . ?
C4 O2 H2 108.5(19) . . ?
Cr1 O3 Cr2 98.90(6) . . ?
C8 O3 Cr1 132.84(14) . . ?
C8 O3 Cr2 111.75(13) . . ?
Cr2 O4 H4 117(2) . . ?
C10 O4 Cr2 116.70(14) . . ?
C10 O4 H4 111.1(19) . . ?
C13 O5 Cr2 127.87(15) . . ?
C13 O6 Cr1 127.90(14) . . ?
C1 N1 Cr1 106.80(14) . . ?
C3 N1 Cr1 104.51(13) . . ?
C3 N1 C1 110.62(17) . . ?
C3 N1 C5 111.12(19) . . ?
C5 N1 Cr1 112.58(13) . . ?
C5 N1 C1 110.96(17) . . ?
C7 N2 Cr2 105.79(14) . . ?
C7 N2 C11A 103.6(7) . . ?
C9 N2 Cr2 104.82(13) . . ?
C9 N2 C7 111.52(18) . . ?
C9 N2 C11 111.9(8) . . ?
C9 N2 C11A 108.5(7) . . ?
C11 N2 Cr2 107.6(4) . . ?
C11 N2 C7 114.4(7) . . ?
C11A N2 Cr2 122.6(4) . . ?
N1 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
N1 C1 C2 110.25(18) . . ?
H1A C1 H1B 108.1 . . ?
C2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
O1 C2 C1 106.95(18) . . ?
O1 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
C1 C2 H2A 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N1 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
N1 C3 C4 110.2(2) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O2 C4 C3 108.04(18) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
N1 C5 H5A 108.5 . . ?
N1 C5 H5B 108.5 . . ?
N1 C5 C6 115.3(2) . . ?
H5A C5 H5B 107.5 . . ?
C6 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.6 . . ?
N2 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 N2 110.06(18) . . ?
C8 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
O3 C8 C7 106.29(18) . . ?
O3 C8 H8A 110.5 . . ?
O3 C8 H8B 110.5 . . ?
C7 C8 H8A 110.5 . . ?
C7 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
N2 C9 H9A 109.6 . . ?
N2 C9 H9B 109.6 . . ?
N2 C9 C10 110.2(2) . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
O4 C10 C9 108.11(19) . . ?
O4 C10 H10A 110.1 . . ?
O4 C10 H10B 110.1 . . ?
C9 C10 H10A 110.1 . . ?
C9 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 H11A 109.2 . . ?
N2 C11 H11B 109.2 . . ?
N2 C11 C12 112.0(7) . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
N2 C11A H11C 107.8 . . ?
N2 C11A H11D 107.8 . . ?
H11C C11A H11D 107.1 . . ?
C12A C11A N2 118.2(9) . . ?
C12A C11A H11C 107.8 . . ?
C12A C11A H11D 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11A C12A H12D 109.5 . . ?
C11A C12A H12E 109.5 . . ?
C11A C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
O5 C13 O6 125.10(19) . . ?
O5 C13 C14 117.8(2) . . ?
O6 C13 C14 117.1(2) . . ?
C15 C14 C13 120.2(2) . . ?
C15 C14 C19 120.0(2) . . ?
C19 C14 C13 119.8(2) . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.5(3) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.5(2) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.2(2) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.2(3) . . ?
C19 C18 H18 119.9 . . ?
C14 C19 H19 120.2 . . ?
C18 C19 C14 119.6(2) . . ?
C18 C19 H19 120.2 . . ?
C20 O7 C20 112.9(3) . 3_656 ?
C20 O7 H20B 117(2) 3_656 . ?
C20 O7 H20B 41.7(12) . . ?
C20 O7 H20C 141(2) 3_656 . ?
C20 O7 H20C 41.0(12) . . ?
H20B O7 H20C 66(2) . . ?
O7 C20 O7 67.1(3) . 3_656 ?
O7 C20 C21 171.2(3) 3_656 . ?
O7 C20 C21 106.5(3) . . ?
O7 C20 C22 171.1(4) . . ?
O7 C20 H20A 118(4) . . ?
O7 C20 H20A 81(4) 3_656 . ?
O7 C20 H20B 70(4) . . ?
O7 C20 H20B 96(4) 3_656 . ?
O7 C20 H20C 126(4) 3_656 . ?
O7 C20 H20C 72(4) . . ?
O7 C20 H20D 120(4) . . ?
O7 C20 H20D 77(4) 3_656 . ?
C21 C20 H20A 108(4) . . ?
C21 C20 H20B 88(3) . . ?
C21 C20 H20C 46(4) . . ?
C21 C20 H20D 102(4) . . ?
C22 C20 O7 107.3(3) . 3_656 ?
C22 C20 C21 78.2(3) . . ?
C22 C20 H20A 67(3) . . ?
C22 C20 H20B 118(4) . . ?
C22 C20 H20C 108(4) . . ?
C22 C20 H20D 52(3) . . ?
H20A C20 H20B 61(4) . . ?
H20A C20 H20C 152(5) . . ?
H20A C20 H20D 102(3) . . ?
H20B C20 H20C 103(3) . . ?
H20B C20 H20D 162(4) . . ?
H20C C20 H20D 94(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
C20 C21 H20C 37.9(11) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21A C21 H20C 133.9 . . ?
H21B C21 H21C 109.5 . . ?
H21B C21 H20C 112.6 . . ?
H21C C21 H20C 73.2 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
C20 C22 H20A 40.2(11) . . ?
C20 C22 H20D 42.4(10) . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22A C22 H20A 86.3 . . ?
H22A C22 H20D 151.3 . . ?
H22B C22 H22C 109.5 . . ?
H22B C22 H20A 149.7 . . ?
H22B C22 H20D 82.1 . . ?
H22C C22 H20A 88.0 . . ?
H22C C22 H20D 89.9 . . ?
H20A C22 H20D 73(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
O2 H2 Cl3 0.817(17) 2.088(17) 2.8960(17) 170(3) .
O4 H4 Cl3 0.817(17) 2.137(17) 2.949(2) 173(3) .

_olex2_date_sample_data_collection 2017-02-09
_olex2_date_sample_submission    2017-02-09
_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 L149o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.796
####################################################################### 
# 
# 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 1579643'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
# local name eb16269

_audit_creation_date             2016-11-24
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H27 Cl2 Cr2 N2 O6, Cl'
_chemical_formula_sum            'C12 H27 Cl3 Cr2 N2 O6'
_chemical_formula_weight         505.70
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl Na'
_chemical_oxdiff_usercomment     '@ 120 K L143 SOB'
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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.10996(16)
_cell_length_b                   10.2978(2)
_cell_length_c                   13.8317(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.201(2)
_cell_angle_gamma                90
_cell_volume                     985.95(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    16411
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      30.9550
_cell_measurement_theta_min      3.5670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
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            'dark green'
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             520
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 5 -2 0.1452
5 1 1 0.1725
-5 0 -2 0.1486
-2 5 -3 0.1475
0 -5 -3 0.0882
-5 -1 5 0.1949
-4 1 5 0.1968
1 5 2 0.1479
2 -5 -5 0.1146
4 0 -5 0.1980
0 -1 1 0.1465
5 3 3 0.1637
-4 0 -5 0.1218
0 1 0 0.1496
-5 1 2 0.1708
0 -4 -5 0.0879
1 -1 -5 0.1460
1 5 5 0.1392
-2 0 5 0.1794
3 3 5 0.1518
0 1 -5 0.1608
0 -1 5 0.1535
0 0 1 0.1488
0 1 5 0.1524

_exptl_crystal_recrystallization_method 
'The material was recrystallised from acetonitrile by hydrothermal bomb'
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.252
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
0.0007 4.9936 -1.9999 0.1427 -0.2307 -0.2364
4.9948 0.9968 0.9993 -0.1693 0.2907 -0.4104
-4.9946 0.0018 -1.9985 0.2292 -0.3340 0.3652
-1.9971 4.9943 -2.9991 0.2449 -0.3633 -0.0897
-0.0002 -4.9950 -2.9937 0.1186 0.2544 0.2538
-4.9954 -0.9952 4.9931 -0.1443 -0.3192 0.3896
-3.9962 1.0020 4.9924 -0.1539 -0.3466 0.2206
0.9993 4.9942 1.9952 -0.0913 -0.1810 -0.3220
1.9979 -4.9964 -4.9908 0.1732 0.4013 0.1174
3.9963 -0.0031 -4.9929 0.1616 0.2985 -0.2692
-0.0002 -0.9986 0.9992 -0.0599 0.0433 0.0452
4.9948 2.9950 2.9957 -0.2586 0.1851 -0.5147
-3.9954 0.0005 -4.9945 0.3611 -0.2510 0.3040
0.0001 0.9988 -0.0005 0.0076 -0.0480 -0.0487
-4.9949 1.0017 1.9960 0.0278 -0.4010 0.3026
0.0000 -3.9967 -4.9917 0.2308 0.2159 0.2121
0.9993 -1.0006 -4.9930 0.2287 0.1405 -0.0056
0.9990 4.9950 4.9914 -0.2481 -0.1952 -0.3324
-1.9984 0.0022 4.9933 -0.2114 -0.1611 0.1259
2.9967 2.9964 4.9928 -0.3132 0.0382 -0.3783
0.0006 0.9975 -4.9942 0.2690 -0.0243 -0.0313
-0.0006 -0.9975 4.9942 -0.2690 0.0243 0.0313
-0.0001 0.0003 0.9987 -0.0523 -0.0047 -0.0035
-0.0004 1.0002 4.9932 -0.2537 -0.0718 -0.0660

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31889
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.252
_diffrn_reflns_theta_min         2.943
_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 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -40.00  57.00   1.00    1.00    --  -13.24  57.00-120.00   97
  2  ω    -20.00  27.00   1.00    1.00    --  -13.24 -99.00-120.00   47
  3  ω    -83.00  13.00   1.00    1.00    --  -13.24 -57.00  90.00   96
  4  ω    -20.00  27.00   1.00    1.00    --  -13.24 -99.00 -60.00   47
  5  ω    -12.00  85.00   1.00    1.00    --   14.65  57.00  30.00   97
  6  ω    -36.00  59.00   1.00    1.00    --  -13.24  38.00   0.00   95
  7  ω    -83.00  13.00   1.00    1.00    --  -13.24 -57.00-150.00   96
  8  ω    -20.00  55.00   1.00    1.00    --   14.65 -99.00   0.00   75
  9  ω    -20.00  55.00   1.00    1.00    --   14.65 -99.00  90.00   75
 10  ω     11.00  79.00   1.00    1.00    --   14.65-141.00 -23.00   68
 11  ω    -20.00  55.00   1.00    1.00    --   14.65 -99.00-180.00   75
 12  ω     34.00 100.00   1.00    1.00    --   14.65-178.00-120.00   66
 13  ω    -56.00  41.00   1.00    1.00    --   14.65 -57.00  30.00   97
 14  ω      5.00  40.00   1.00    1.00    --   14.65-129.00 148.00   35
;
_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      -0.0249542000
_diffrn_orient_matrix_UB_12      0.0076275000
_diffrn_orient_matrix_UB_13      -0.0523366000
_diffrn_orient_matrix_UB_21      0.0687479000
_diffrn_orient_matrix_UB_22      -0.0480999000
_diffrn_orient_matrix_UB_23      -0.0047351000
_diffrn_orient_matrix_UB_31      -0.0717459000
_diffrn_orient_matrix_UB_32      -0.0487277000
_diffrn_orient_matrix_UB_33      -0.0034705000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                5674
_reflns_number_total             5981
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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         0.347
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 
;
 Flack x determined using 2474 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         5981
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0274
_refine_ls_restrained_S_all      1.057
_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)+(0.0211P)²+0.2665P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0582
_refine_special_details          
;
O-bound H atoms were identified from a difference Fourier map and freely refined.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          4 Report

Not significant

#===============================================================================
720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          3 Note
791_ALERT_4_G The Model has Chirality at N1      (Chiral SPGR)          R Verify
791_ALERT_4_G The Model has Chirality at N2      (Chiral SPGR)          R Verify
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           2 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        157 Note
978_ALERT_2_G Number C-C Bonds with Positive Residual Density           4 Note


Not significant
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1AA(H1AA,H1AB), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,
 H6B), C7(H7A,H7B), C8(H8A,H8B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_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 0.22878(6) 0.77315(4) 0.25391(3) 0.00977(9) Uani 1 1 d . . . . .
Cr2 Cr 0.20642(6) 1.06087(4) 0.25630(3) 0.00893(9) Uani 1 1 d . . . . .
Cl1 Cl 0.42572(10) 0.61112(7) 0.33801(5) 0.01863(15) Uani 1 1 d . . . . .
Cl2 Cl -0.02442(9) 1.22117(6) 0.22568(5) 0.01579(13) Uani 1 1 d . . . . .
Cl3 Cl 0.40139(9) 0.93605(7) -0.00321(5) 0.01615(14) Uani 1 1 d . . . . .
O1 O 0.0632(2) 0.9131(2) 0.18647(12) 0.0110(3) Uani 1 1 d . . . . .
O2 O 0.3213(3) 0.7309(2) 0.13106(15) 0.0136(4) Uani 1 1 d . . . . .
O3 O 0.4035(2) 0.9227(2) 0.28414(12) 0.0107(3) Uani 1 1 d . . . . .
O4 O 0.2925(3) 1.1181(2) 0.13495(15) 0.0124(4) Uani 1 1 d . . . . .
O5 O 0.1281(3) 0.80121(19) 0.37498(15) 0.0145(4) Uani 1 1 d . . . . .
O6 O 0.1304(3) 1.01934(19) 0.38183(15) 0.0135(4) Uani 1 1 d . . . . .
N1 N -0.0033(3) 0.6564(2) 0.18266(17) 0.0127(5) Uani 1 1 d . . . . .
N2 N 0.4398(3) 1.1774(2) 0.32738(17) 0.0116(4) Uani 1 1 d . . . . .
C1 C -0.1518(4) 0.7451(3) 0.1202(2) 0.0161(6) Uani 1 1 d . . . . .
H1A H -0.283021 0.709454 0.115245 0.019 Uiso 1 1 calc R . . . .
H1B H -0.129225 0.751695 0.052356 0.019 Uiso 1 1 calc R . . . .
C1AA C 0.5476(4) 0.9527(2) 0.3719(2) 0.0142(5) Uani 1 1 d . . . . .
H1AA H 0.658046 0.892078 0.379192 0.017 Uiso 1 1 calc R . . . .
H1AB H 0.493112 0.945404 0.431411 0.017 Uiso 1 1 calc R . . . .
C2 C -0.1358(4) 0.8783(3) 0.1682(2) 0.0145(5) Uani 1 1 d . . . . .
H2A H -0.216028 0.942055 0.123330 0.017 Uiso 1 1 calc R . . . .
H2B H -0.179585 0.875359 0.231195 0.017 Uiso 1 1 calc R . . . .
C3 C 0.0805(4) 0.5655(3) 0.1190(2) 0.0164(5) Uani 1 1 d . . . . .
H3A H -0.025161 0.520620 0.071735 0.020 Uiso 1 1 calc R . . . .
H3B H 0.160047 0.498932 0.161183 0.020 Uiso 1 1 calc R . . . .
C4 C 0.2038(4) 0.6398(3) 0.0621(2) 0.0189(6) Uani 1 1 d . . . . .
H4A H 0.287597 0.579301 0.035369 0.023 Uiso 1 1 calc R . . . .
H4B H 0.120989 0.687159 0.005914 0.023 Uiso 1 1 calc R . . . .
C5 C -0.0931(4) 0.5794(3) 0.2506(2) 0.0211(6) Uani 1 1 d . . . . .
H5A H 0.006632 0.528956 0.295713 0.032 Uiso 1 1 calc GR . . . .
H5B H -0.189540 0.520348 0.211797 0.032 Uiso 1 1 calc GR . . . .
H5C H -0.155946 0.638120 0.289332 0.032 Uiso 1 1 calc GR . . . .
C6 C 0.6130(4) 1.0913(3) 0.3600(2) 0.0165(6) Uani 1 1 d . . . . .
H6A H 0.692590 1.122821 0.424037 0.020 Uiso 1 1 calc R . . . .
H6B H 0.693075 1.093802 0.310160 0.020 Uiso 1 1 calc R . . . .
C7 C 0.4706(4) 1.2706(3) 0.2494(2) 0.0151(5) Uani 1 1 d . . . . .
H7A H 0.597838 1.313435 0.271426 0.018 Uiso 1 1 calc R . . . .
H7B H 0.369446 1.338479 0.238896 0.018 Uiso 1 1 calc R . . . .
C8 C 0.4628(4) 1.1993(3) 0.1539(2) 0.0201(6) Uani 1 1 d . . . . .
H8A H 0.455941 1.261791 0.098776 0.024 Uiso 1 1 calc R . . . .
H8B H 0.580019 1.145349 0.159401 0.024 Uiso 1 1 calc R . . . .
C9 C 0.4035(4) 1.2517(3) 0.4129(2) 0.0187(6) Uani 1 1 d . . . . .
H9A H 0.285364 1.303237 0.391598 0.028 Uiso 1 1 calc GR . . . .
H9B H 0.512837 1.309723 0.438399 0.028 Uiso 1 1 calc GR . . . .
H9C H 0.388125 1.191422 0.465401 0.028 Uiso 1 1 calc GR . . . .
C10 C 0.1082(3) 0.9081(3) 0.41638(18) 0.0137(5) Uani 1 1 d . . . . .
C11 C 0.0587(4) 0.9044(3) 0.51673(19) 0.0198(6) Uani 1 1 d . . . . .
H11A H 0.170414 0.933116 0.567733 0.030 Uiso 1 1 calc GR . . . .
H11B H 0.024395 0.815468 0.531235 0.030 Uiso 1 1 calc GR . . . .
H11C H -0.050996 0.962160 0.516420 0.030 Uiso 1 1 calc GR . . . .
H4 H 0.311(6) 1.060(4) 0.093(3) 0.034(11) Uiso 1 1 d . . . . .
H2 H 0.348(6) 0.790(4) 0.101(3) 0.035(12) Uiso 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 2.3139(8) . ?
Cr1 O1 1.9573(19) . ?
Cr1 O2 2.005(2) . ?
Cr1 O3 1.9628(19) . ?
Cr1 O5 1.987(2) . ?
Cr1 N1 2.097(2) . ?
Cr2 Cl2 2.2979(7) . ?
Cr2 O1 1.9587(19) . ?
Cr2 O3 1.9720(19) . ?
Cr2 O4 2.002(2) . ?
Cr2 O6 1.980(2) . ?
Cr2 N2 2.101(2) . ?
O1 C2 1.425(3) . ?
O2 C4 1.457(3) . ?
O2 H2 0.79(4) . ?
O3 C1AA 1.432(3) . ?
O4 C8 1.446(3) . ?
O4 H4 0.87(4) . ?
O5 C10 1.264(4) . ?
O6 C10 1.265(4) . ?
N1 C1 1.510(3) . ?
N1 C3 1.499(4) . ?
N1 C5 1.481(4) . ?
N2 C6 1.500(3) . ?
N2 C7 1.497(4) . ?
N2 C9 1.481(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.517(4) . ?
C1AA H1AA 0.9900 . ?
C1AA H1AB 0.9900 . ?
C1AA C6 1.521(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.512(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.501(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.508(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
O1 Cr1 Cl1 178.30(6) . . ?
O1 Cr1 O2 91.94(8) . . ?
O1 Cr1 O3 78.83(8) . . ?
O1 Cr1 O5 90.08(8) . . ?
O1 Cr1 N1 82.83(8) . . ?
O2 Cr1 Cl1 89.52(6) . . ?
O2 Cr1 N1 81.52(9) . . ?
O3 Cr1 Cl1 100.25(6) . . ?
O3 Cr1 O2 92.10(8) . . ?
O3 Cr1 O5 92.22(8) . . ?
O3 Cr1 N1 160.37(8) . . ?
O5 Cr1 Cl1 88.53(6) . . ?
O5 Cr1 O2 175.52(9) . . ?
O5 Cr1 N1 94.77(9) . . ?
N1 Cr1 Cl1 98.26(7) . . ?
O1 Cr2 Cl2 101.43(6) . . ?
O1 Cr2 O3 78.58(8) . . ?
O1 Cr2 O4 92.24(8) . . ?
O1 Cr2 O6 92.82(8) . . ?
O1 Cr2 N2 160.13(8) . . ?
O3 Cr2 Cl2 179.27(6) . . ?
O3 Cr2 O4 92.09(8) . . ?
O3 Cr2 O6 89.83(8) . . ?
O3 Cr2 N2 82.56(8) . . ?
O4 Cr2 Cl2 88.64(6) . . ?
O4 Cr2 N2 82.21(9) . . ?
O6 Cr2 Cl2 89.44(6) . . ?
O6 Cr2 O4 174.85(8) . . ?
O6 Cr2 N2 93.30(9) . . ?
N2 Cr2 Cl2 97.51(7) . . ?
Cr1 O1 Cr2 98.55(7) . . ?
C2 O1 Cr1 111.35(16) . . ?
C2 O1 Cr2 131.76(16) . . ?
Cr1 O2 H2 116(3) . . ?
C4 O2 Cr1 116.38(17) . . ?
C4 O2 H2 109(3) . . ?
Cr1 O3 Cr2 97.91(7) . . ?
C1AA O3 Cr1 130.20(16) . . ?
C1AA O3 Cr2 110.43(16) . . ?
Cr2 O4 H4 119(3) . . ?
C8 O4 Cr2 114.98(16) . . ?
C8 O4 H4 106(3) . . ?
C10 O5 Cr1 127.42(18) . . ?
C10 O6 Cr2 127.56(18) . . ?
C1 N1 Cr1 107.13(16) . . ?
C3 N1 Cr1 104.99(16) . . ?
C3 N1 C1 111.2(2) . . ?
C5 N1 Cr1 114.55(17) . . ?
C5 N1 C1 109.9(2) . . ?
C5 N1 C3 109.0(2) . . ?
C6 N2 Cr2 108.05(16) . . ?
C7 N2 Cr2 104.98(16) . . ?
C7 N2 C6 110.5(2) . . ?
C9 N2 Cr2 113.94(17) . . ?
C9 N2 C6 110.2(2) . . ?
C9 N2 C7 109.0(2) . . ?
N1 C1 H1A 109.9 . . ?
N1 C1 H1B 109.9 . . ?
N1 C1 C2 108.9(2) . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
O3 C1AA H1AA 110.4 . . ?
O3 C1AA H1AB 110.4 . . ?
O3 C1AA C6 106.8(2) . . ?
H1AA C1AA H1AB 108.6 . . ?
C6 C1AA H1AA 110.4 . . ?
C6 C1AA H1AB 110.4 . . ?
O1 C2 C1 106.1(2) . . ?
O1 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N1 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
N1 C3 C4 110.2(2) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O2 C4 C3 107.4(2) . . ?
O2 C4 H4A 110.2 . . ?
O2 C4 H4B 110.2 . . ?
C3 C4 H4A 110.2 . . ?
C3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C1AA 109.7(2) . . ?
N2 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
C1AA C6 H6A 109.7 . . ?
C1AA C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 H7A 109.7 . . ?
N2 C7 H7B 109.7 . . ?
N2 C7 C8 109.8(2) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.7 . . ?
C8 C7 H7B 109.7 . . ?
O4 C8 C7 107.7(2) . . ?
O4 C8 H8A 110.2 . . ?
O4 C8 H8B 110.2 . . ?
C7 C8 H8A 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5 C10 O6 125.5(2) . . ?
O5 C10 C11 117.9(3) . . ?
O6 C10 C11 116.5(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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 C2 C1 -49.5(2) . . . . ?
Cr1 O2 C4 C3 -19.6(3) . . . . ?
Cr1 O3 C1AA C6 -170.41(16) . . . . ?
Cr1 O5 C10 O6 8.0(4) . . . . ?
Cr1 O5 C10 C11 -170.45(17) . . . . ?
Cr1 N1 C1 C2 -28.8(3) . . . . ?
Cr1 N1 C3 C4 -46.6(2) . . . . ?
Cr2 O1 C2 C1 -173.76(17) . . . . ?
Cr2 O3 C1AA C6 -49.9(2) . . . . ?
Cr2 O4 C8 C7 -27.7(3) . . . . ?
Cr2 O6 C10 O5 -1.3(4) . . . . ?
Cr2 O6 C10 C11 177.13(17) . . . . ?
Cr2 N2 C6 C1AA -24.0(3) . . . . ?
Cr2 N2 C7 C8 -44.8(2) . . . . ?
O3 C1AA C6 N2 47.9(3) . . . . ?
N1 C1 C2 O1 50.7(3) . . . . ?
N1 C3 C4 O2 44.0(3) . . . . ?
N2 C7 C8 O4 48.2(3) . . . . ?
C1 N1 C3 C4 68.9(3) . . . . ?
C3 N1 C1 C2 -143.0(2) . . . . ?
C5 N1 C1 C2 96.2(3) . . . . ?
C5 N1 C3 C4 -169.8(2) . . . . ?
C6 N2 C7 C8 71.5(3) . . . . ?
C7 N2 C6 C1AA -138.4(2) . . . . ?
C9 N2 C6 C1AA 101.1(3) . . . . ?
C9 N2 C7 C8 -167.2(2) . . . . ?

_shelx_SHELXL_version_number     2016/6
_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 'L143 SOB'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.360
_oxdiff_exptl_absorpt_empirical_full_min 0.806
####################################################################### 
# 
# 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 1579648'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;

#  local name eb17027

_audit_creation_date             2017-02-21
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H39 Cl2 Cr2 N2 O6, Cl'
_chemical_formula_sum            'C22 H39 Cl3 Cr2 N2 O6'
_chemical_formula_weight         637.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H39 Cl3 Cr2 N2 O6'
_chemical_oxdiff_usercomment     '@ 120 K L232o L-IPA'
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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.0888(6)
_cell_length_b                   10.2661(4)
_cell_length_c                   39.2028(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5670.2(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6388
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      24.7780
_cell_measurement_theta_min      3.5620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0082
0 5 2 0.1701
-5 1 1 0.1661
0 0 1 0.0082
-1 -5 -1 0.2086
5 -5 -2 0.1988
5 -1 -1 0.1495
-5 0 1 0.1813

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of acetonitrile and isopropanol by solvent layering'
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.316
_exptl_crystal_size_min          0.016
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
-0.0000 0.0001 -1.0001 0.0181 -0.0002 0.0000
0.0008 4.9994 2.0163 -0.0328 0.2971 0.1770
-5.0017 0.9984 1.0069 -0.0150 0.1887 -0.1807
0.0000 -0.0001 1.0001 -0.0181 0.0002 -0.0000
-1.0012 -4.9998 -1.0154 0.0152 -0.2710 -0.2202
5.0010 -4.9979 -2.0198 0.0304 -0.4263 0.0391
5.0017 -0.9984 -1.0069 0.0150 -0.1887 0.1807
-5.0018 -0.0016 1.0037 -0.0157 0.1294 -0.2161

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            41273
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.892
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00   2.00   1.00   25.00    --   -7.39 -38.00 -90.00   34
  2  ω    -72.00   4.00   1.00   25.00    --   -7.39 -57.00 150.00   76
  3  ω    -12.00  14.00   1.00   25.00    --   -7.39 -99.00   0.00   26
  4  ω     35.00  68.00   1.00   25.00    --    8.80-160.00 160.32   33
  5  ω      3.00  84.00   1.00   25.00    --    8.80  19.00 -60.00   81
  6  ω    -19.00   9.00   1.00   25.00    --    8.80 -99.00-150.00   28
  7  ω      0.00  27.00   1.00   25.00    --    8.80 -99.00  60.00   27
;
_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      -0.0004928000
_diffrn_orient_matrix_UB_12      0.0007370000
_diffrn_orient_matrix_UB_13      -0.0180955000
_diffrn_orient_matrix_UB_21      -0.0258400000
_diffrn_orient_matrix_UB_22      0.0593345000
_diffrn_orient_matrix_UB_23      0.0002522000
_diffrn_orient_matrix_UB_31      0.0431843000
_diffrn_orient_matrix_UB_32      0.0354084000
_diffrn_orient_matrix_UB_33      -0.0000388000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3810
_reflns_number_total             5174
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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         0.490
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5174
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0522
_refine_ls_restrained_S_all      0.933
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1536
_refine_special_details          
;
O-bound H atoms were identified from a difference Fourier map and refined freely.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
220_ALERT_2_C Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        5.7 Ratio
222_ALERT_3_C Non-Solvent Resd 1   H Uiso(max)/Uiso(min) Range        7.0 Ratio
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00775 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      6.058 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           6 Note
978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note

Not significant

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          4 Note
020_ALERT_3_G The value of Rint is greater than 0.12 .........      0.128 Report
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
793_ALERT_4_G The Model has Chirality at N1      (Centro SPGR)          S Verify
793_ALERT_4_G The Model has Chirality at N2      (Centro SPGR)          S Verify
860_ALERT_3_G Number of Least-Squares Restraints .............          2 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
955_ALERT_1_G Reported (CIF) and Actual (FCF) Lmax Differ by .          1 Units

Not significant
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2 = O4-H4
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_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 0.47808(5) 0.38246(6) 0.33379(2) 0.0135(2) Uani 1 1 d . . . . .
Cr2 Cr 0.50925(5) 0.66543(7) 0.34187(2) 0.0133(2) Uani 1 1 d . . . . .
Cl1 Cl 0.39608(8) 0.21882(10) 0.36187(3) 0.0226(3) Uani 1 1 d . . . . .
Cl2 Cl 0.63008(8) 0.80960(10) 0.33168(3) 0.0211(3) Uani 1 1 d . . . . .
O1 O 0.55099(19) 0.5234(3) 0.31280(7) 0.0148(6) Uani 1 1 d . . . . .
O2 O 0.3905(2) 0.3665(3) 0.29411(8) 0.0185(7) Uani 1 1 d D . . . .
H2 H 0.361(3) 0.434(3) 0.2897(12) 0.022 Uiso 1 1 d DR . . . .
O3 O 0.41061(19) 0.5361(3) 0.35042(8) 0.0156(6) Uani 1 1 d . . . . .
O4 O 0.4333(2) 0.7483(3) 0.30382(8) 0.0197(7) Uani 1 1 d D . . . .
H4 H 0.387(2) 0.707(4) 0.2967(12) 0.024 Uiso 1 1 d DR . . . .
O5 O 0.5675(2) 0.3850(3) 0.37304(8) 0.0185(7) Uani 1 1 d . . . . .
O6 O 0.5742(2) 0.6009(3) 0.38293(8) 0.0224(7) Uani 1 1 d . . . . .
N1 N 0.5647(2) 0.2670(3) 0.30289(9) 0.0163(8) Uani 1 1 d . . . . .
N2 N 0.4196(3) 0.7829(3) 0.37251(10) 0.0224(9) Uani 1 1 d . . . . .
C1 C 0.6320(3) 0.3564(4) 0.28398(12) 0.0183(10) Uani 1 1 d . . . . .
H1A H 0.694038 0.312699 0.280879 0.022 Uiso 1 1 calc R . . . .
H1B H 0.605899 0.376894 0.261160 0.022 Uiso 1 1 calc R . . . .
C2 C 0.6451(3) 0.4804(4) 0.30410(12) 0.0172(9) Uani 1 1 d . . . . .
H2A H 0.682812 0.463746 0.324960 0.021 Uiso 1 1 calc R . . . .
H2B H 0.678121 0.546923 0.290204 0.021 Uiso 1 1 calc R . . . .
C3 C 0.4970(3) 0.2005(4) 0.27878(12) 0.0196(10) Uani 1 1 d . . . . .
H3A H 0.462376 0.130626 0.290967 0.023 Uiso 1 1 calc R . . . .
H3B H 0.532890 0.160247 0.259796 0.023 Uiso 1 1 calc R . . . .
C4 C 0.4273(3) 0.2986(4) 0.26481(11) 0.0199(10) Uani 1 1 d . . . . .
H4A H 0.459440 0.359887 0.249114 0.024 Uiso 1 1 calc R . . . .
H4B H 0.375521 0.254206 0.252301 0.024 Uiso 1 1 calc R . . . .
C5 C 0.6201(3) 0.1671(4) 0.32192(13) 0.0232(10) Uani 1 1 d . . . . .
H5A H 0.667346 0.210417 0.336352 0.035 Uiso 1 1 calc GR . . . .
H5B H 0.652367 0.109563 0.305694 0.035 Uiso 1 1 calc GR . . . .
H5C H 0.577116 0.115724 0.336230 0.035 Uiso 1 1 calc GR . . . .
C6 C 0.3664(3) 0.6863(4) 0.39391(12) 0.0237(11) Uani 1 1 d . . . . .
H6A H 0.310110 0.728898 0.404097 0.028 Uiso 1 1 calc R . . . .
H6B H 0.407647 0.655589 0.412717 0.028 Uiso 1 1 calc R . . . .
C7 C 0.3350(3) 0.5708(4) 0.37242(12) 0.0247(11) Uani 1 1 d . . . . .
H7A H 0.318561 0.496355 0.387355 0.030 Uiso 1 1 calc R . . . .
H7B H 0.278227 0.594223 0.358880 0.030 Uiso 1 1 calc R . . . .
C8 C 0.3521(3) 0.8529(5) 0.34898(14) 0.0281(12) Uani 1 1 d . . . . .
H8A H 0.293152 0.801290 0.346428 0.034 Uiso 1 1 calc R . . . .
H8B H 0.335003 0.938453 0.358919 0.034 Uiso 1 1 calc R . . . .
C9 C 0.3964(3) 0.8724(4) 0.31517(13) 0.0260(11) Uani 1 1 d . . . . .
H9A H 0.348772 0.905290 0.298721 0.031 Uiso 1 1 calc R . . . .
H9B H 0.448407 0.936894 0.316834 0.031 Uiso 1 1 calc R . . . .
C10 C 0.4700(4) 0.8756(5) 0.39481(14) 0.0324(12) Uani 1 1 d . . . . .
H10A H 0.517342 0.828744 0.408412 0.049 Uiso 1 1 calc GR . . . .
H10B H 0.424404 0.918151 0.410048 0.049 Uiso 1 1 calc GR . . . .
H10C H 0.501773 0.941531 0.380794 0.049 Uiso 1 1 calc GR . . . .
C11 C 0.5884(3) 0.4841(4) 0.39113(11) 0.0197(10) Uani 1 1 d . . . . .
C12 C 0.6334(3) 0.4576(5) 0.42519(13) 0.0268(11) Uani 1 1 d . . . . .
C13 C 0.5786(4) 0.3985(5) 0.45058(13) 0.0338(13) Uani 1 1 d . . . . .
C14 C 0.6206(5) 0.3747(6) 0.48212(14) 0.0422(15) Uani 1 1 d . . . . .
C15 C 0.7164(5) 0.4099(6) 0.48789(15) 0.0503(16) Uani 1 1 d . . . . .
C16 C 0.7698(4) 0.4707(6) 0.46224(15) 0.0452(15) Uani 1 1 d . . . . .
C17 C 0.7273(4) 0.4978(5) 0.43070(13) 0.0333(12) Uani 1 1 d . . . . .
C18 C 0.4758(4) 0.3618(6) 0.44434(15) 0.0448(15) Uani 1 1 d . . . . .
H18A H 0.470835 0.267169 0.441541 0.067 Uiso 1 1 calc GR . . . .
H18B H 0.453054 0.405100 0.423627 0.067 Uiso 1 1 calc GR . . . .
H18C H 0.437168 0.389307 0.463836 0.067 Uiso 1 1 calc GR . . . .
C19 C 0.5610(5) 0.3132(7) 0.51052(16) 0.0593(19) Uani 1 1 d . . . . .
H19A H 0.530641 0.382070 0.523968 0.089 Uiso 1 1 calc GR . . . .
H19B H 0.602044 0.260948 0.525340 0.089 Uiso 1 1 calc GR . . . .
H19C H 0.512114 0.257298 0.500420 0.089 Uiso 1 1 calc GR . . . .
C20 C 0.7610(6) 0.3823(10) 0.52246(19) 0.097(3) Uani 1 1 d . . . . .
H20A H 0.730178 0.436046 0.539890 0.146 Uiso 1 1 calc GR . . . .
H20B H 0.828868 0.402922 0.521635 0.146 Uiso 1 1 calc GR . . . .
H20C H 0.752686 0.289992 0.528137 0.146 Uiso 1 1 calc GR . . . .
C21 C 0.8737(4) 0.5065(8) 0.46791(18) 0.066(2) Uani 1 1 d . . . . .
H21A H 0.911807 0.426845 0.469470 0.099 Uiso 1 1 calc GR . . . .
H21B H 0.879845 0.556219 0.489134 0.099 Uiso 1 1 calc GR . . . .
H21C H 0.896303 0.559466 0.448752 0.099 Uiso 1 1 calc GR . . . .
C22 C 0.7837(4) 0.5643(6) 0.40232(14) 0.0407(14) Uani 1 1 d . . . . .
H22A H 0.832708 0.504807 0.393896 0.061 Uiso 1 1 calc GR . . . .
H22B H 0.813632 0.643401 0.411280 0.061 Uiso 1 1 calc GR . . . .
H22C H 0.740772 0.587479 0.383597 0.061 Uiso 1 1 calc GR . . . .
Cl3 Cl 0.27891(8) 0.59456(10) 0.27289(3) 0.0216(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 2.3171(12) . ?
Cr1 O1 1.956(3) . ?
Cr1 O2 1.992(3) . ?
Cr1 O3 1.954(3) . ?
Cr1 O5 1.989(3) . ?
Cr1 N1 2.088(3) . ?
Cr2 Cl2 2.2909(12) . ?
Cr2 O1 1.942(3) . ?
Cr2 O3 1.951(3) . ?
Cr2 O4 2.024(3) . ?
Cr2 O6 1.966(3) . ?
Cr2 N2 2.119(4) . ?
O1 C2 1.438(5) . ?
O2 H2 0.826(19) . ?
O2 C4 1.441(5) . ?
O3 C7 1.416(5) . ?
O4 H4 0.825(19) . ?
O4 C9 1.446(5) . ?
O5 C11 1.274(5) . ?
O6 C11 1.257(5) . ?
N1 C1 1.514(5) . ?
N1 C3 1.506(6) . ?
N1 C5 1.489(5) . ?
N2 C6 1.499(6) . ?
N2 C8 1.508(6) . ?
N2 C10 1.475(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.509(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.509(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.521(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.479(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.503(7) . ?
C12 C13 1.398(7) . ?
C12 C17 1.403(7) . ?
C13 C14 1.393(7) . ?
C13 C18 1.516(8) . ?
C14 C15 1.416(9) . ?
C14 C19 1.530(8) . ?
C15 C16 1.403(9) . ?
C15 C20 1.520(9) . ?
C16 C17 1.402(7) . ?
C16 C21 1.525(8) . ?
C17 C22 1.528(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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
O1 Cr1 Cl1 176.43(10) . . ?
O1 Cr1 O2 93.31(12) . . ?
O1 Cr1 O5 89.02(12) . . ?
O1 Cr1 N1 82.48(13) . . ?
O2 Cr1 Cl1 90.14(9) . . ?
O2 Cr1 N1 82.09(13) . . ?
O3 Cr1 Cl1 100.61(9) . . ?
O3 Cr1 O1 78.39(12) . . ?
O3 Cr1 O2 91.46(12) . . ?
O3 Cr1 O5 92.26(12) . . ?
O3 Cr1 N1 159.42(13) . . ?
O5 Cr1 Cl1 87.59(9) . . ?
O5 Cr1 O2 175.95(12) . . ?
O5 Cr1 N1 94.93(13) . . ?
N1 Cr1 Cl1 98.94(10) . . ?
O1 Cr2 Cl2 99.08(9) . . ?
O1 Cr2 O3 78.78(12) . . ?
O1 Cr2 O4 92.48(12) . . ?
O1 Cr2 O6 94.95(12) . . ?
O1 Cr2 N2 160.10(13) . . ?
O3 Cr2 Cl2 177.35(9) . . ?
O3 Cr2 O4 92.06(12) . . ?
O3 Cr2 O6 87.77(12) . . ?
O3 Cr2 N2 82.26(13) . . ?
O4 Cr2 Cl2 89.60(9) . . ?
O4 Cr2 N2 82.15(14) . . ?
O6 Cr2 Cl2 90.86(10) . . ?
O6 Cr2 O4 172.39(13) . . ?
O6 Cr2 N2 90.28(15) . . ?
N2 Cr2 Cl2 100.03(11) . . ?
Cr2 O1 Cr1 98.60(13) . . ?
C2 O1 Cr1 110.9(2) . . ?
C2 O1 Cr2 130.4(2) . . ?
Cr1 O2 H2 114(3) . . ?
C4 O2 Cr1 116.0(2) . . ?
C4 O2 H2 115(3) . . ?
Cr2 O3 Cr1 98.37(12) . . ?
C7 O3 Cr1 140.6(3) . . ?
C7 O3 Cr2 118.0(2) . . ?
Cr2 O4 H4 117(3) . . ?
C9 O4 Cr2 109.5(3) . . ?
C9 O4 H4 106(3) . . ?
C11 O5 Cr1 126.0(3) . . ?
C11 O6 Cr2 127.2(3) . . ?
C1 N1 Cr1 107.8(2) . . ?
C3 N1 Cr1 104.6(2) . . ?
C3 N1 C1 111.4(3) . . ?
C5 N1 Cr1 114.0(3) . . ?
C5 N1 C1 109.5(3) . . ?
C5 N1 C3 109.5(3) . . ?
C6 N2 Cr2 103.8(3) . . ?
C6 N2 C8 110.0(4) . . ?
C8 N2 Cr2 107.5(3) . . ?
C10 N2 Cr2 114.6(3) . . ?
C10 N2 C6 109.6(4) . . ?
C10 N2 C8 111.0(4) . . ?
N1 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 N1 109.4(3) . . ?
C2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
O1 C2 C1 105.7(3) . . ?
O1 C2 H2A 110.6 . . ?
O1 C2 H2B 110.6 . . ?
C1 C2 H2A 110.6 . . ?
C1 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
N1 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
N1 C3 C4 109.7(3) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
O2 C4 C3 105.5(4) . . ?
O2 C4 H4A 110.6 . . ?
O2 C4 H4B 110.6 . . ?
C3 C4 H4A 110.6 . . ?
C3 C4 H4B 110.6 . . ?
H4A C4 H4B 108.8 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 C7 110.6(4) . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
O3 C7 C6 108.3(4) . . ?
O3 C7 H7A 110.0 . . ?
O3 C7 H7B 110.0 . . ?
C6 C7 H7A 110.0 . . ?
C6 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
N2 C8 H8A 109.6 . . ?
N2 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C9 C8 N2 110.3(4) . . ?
C9 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
O4 C9 C8 108.0(4) . . ?
O4 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C8 C9 H9A 110.1 . . ?
C8 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 C12 116.6(4) . . ?
O6 C11 O5 125.6(4) . . ?
O6 C11 C12 117.8(4) . . ?
C13 C12 C11 118.6(4) . . ?
C13 C12 C17 122.6(5) . . ?
C17 C12 C11 118.8(4) . . ?
C12 C13 C18 121.4(5) . . ?
C14 C13 C12 118.3(5) . . ?
C14 C13 C18 120.3(5) . . ?
C13 C14 C15 120.1(5) . . ?
C13 C14 C19 119.0(6) . . ?
C15 C14 C19 120.8(5) . . ?
C14 C15 C20 119.3(6) . . ?
C16 C15 C14 120.7(5) . . ?
C16 C15 C20 120.0(6) . . ?
C15 C16 C21 121.2(6) . . ?
C17 C16 C15 119.4(5) . . ?
C17 C16 C21 119.4(6) . . ?
C12 C17 C22 120.6(5) . . ?
C16 C17 C12 118.8(5) . . ?
C16 C17 C22 120.6(5) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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 C2 C1 51.1(4) . . . . ?
Cr1 O2 C4 C3 30.0(4) . . . . ?
Cr1 O3 C7 C6 135.5(4) . . . . ?
Cr1 O5 C11 O6 -17.5(6) . . . . ?
Cr1 O5 C11 C12 162.2(3) . . . . ?
Cr1 N1 C1 C2 25.2(4) . . . . ?
Cr1 N1 C3 C4 46.0(4) . . . . ?
Cr2 O1 C2 C1 173.5(3) . . . . ?
Cr2 O3 C7 C6 -19.4(5) . . . . ?
Cr2 O4 C9 C8 -48.3(4) . . . . ?
Cr2 O6 C11 O5 4.2(6) . . . . ?
Cr2 O6 C11 C12 -175.5(3) . . . . ?
Cr2 N2 C6 C7 -42.7(4) . . . . ?
Cr2 N2 C8 C9 -28.4(4) . . . . ?
O5 C11 C12 C13 -68.2(6) . . . . ?
O5 C11 C12 C17 114.3(5) . . . . ?
O6 C11 C12 C13 111.5(5) . . . . ?
O6 C11 C12 C17 -66.0(6) . . . . ?
N1 C1 C2 O1 -48.9(4) . . . . ?
N1 C3 C4 O2 -50.1(4) . . . . ?
N2 C6 C7 O3 41.9(5) . . . . ?
N2 C8 C9 O4 50.7(5) . . . . ?
C1 N1 C3 C4 -70.2(4) . . . . ?
C3 N1 C1 C2 139.4(4) . . . . ?
C5 N1 C1 C2 -99.3(4) . . . . ?
C5 N1 C3 C4 168.5(4) . . . . ?
C6 N2 C8 C9 -140.8(4) . . . . ?
C8 N2 C6 C7 72.1(5) . . . . ?
C10 N2 C6 C7 -165.6(4) . . . . ?
C10 N2 C8 C9 97.7(5) . . . . ?
C11 C12 C13 C14 -179.8(4) . . . . ?
C11 C12 C13 C18 -0.2(7) . . . . ?
C11 C12 C17 C16 -178.7(5) . . . . ?
C11 C12 C17 C22 -1.5(7) . . . . ?
C12 C13 C14 C15 -0.1(8) . . . . ?
C12 C13 C14 C19 178.5(5) . . . . ?
C13 C12 C17 C16 4.0(8) . . . . ?
C13 C12 C17 C22 -178.8(5) . . . . ?
C13 C14 C15 C16 1.0(9) . . . . ?
C13 C14 C15 C20 -179.7(6) . . . . ?
C14 C15 C16 C17 0.6(9) . . . . ?
C14 C15 C16 C21 -178.7(6) . . . . ?
C15 C16 C17 C12 -2.9(9) . . . . ?
C15 C16 C17 C22 179.8(6) . . . . ?
C17 C12 C13 C14 -2.4(8) . . . . ?
C17 C12 C13 C18 177.1(5) . . . . ?
C18 C13 C14 C15 -179.6(6) . . . . ?
C18 C13 C14 C19 -1.1(8) . . . . ?
C19 C14 C15 C16 -177.6(6) . . . . ?
C19 C14 C15 C20 1.8(10) . . . . ?
C20 C15 C16 C17 -178.8(7) . . . . ?
C20 C15 C16 C21 1.9(10) . . . . ?
C21 C16 C17 C12 176.4(5) . . . . ?
C21 C16 C17 C22 -0.9(9) . . . . ?

_olex2_date_sample_data_collection 2017-02-20
_olex2_date_sample_submission    2017-02-14
_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 'L232o L-IPA'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.876
####################################################################### 
# 
# 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 1579649'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT410_8                   
;
PROBLEM: Short Intra H...H Contact   H11A   ..  H9B     .       1.85 Ang.
RESPONSE: Please see the _refine_special_details section of the CIF.
;
_vrf_PLAT410_8_2                 
;
PROBLEM: Short Intra H...H Contact   H7A    ..  H11B    .       1.95 Ang.
RESPONSE: Please see the _refine_special_details section of the CIF.
;
# Added during the CSD deposition process: Thursday 12 October 2017 12:17 PM
# end Validation Reply Form

# local name eb16256
_audit_creation_date             2016-11-14
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C13 H29 Cl2 Cr2 N2 O6, Cl'
_chemical_formula_sum            'C13 H29 Cl3 Cr2 N2 O6'
_chemical_formula_weight         519.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl'
_chemical_oxdiff_usercomment     '@ 120 K L35o'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.5711(3)
_cell_length_b                   13.2720(3)
_cell_length_c                   13.6565(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.948(2)
_cell_angle_gamma                90
_cell_volume                     2096.96(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17733
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.4100
_cell_measurement_theta_min      3.3710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
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            'dark green'
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 5 -7 0.1477
-15 7 -4 0.1183
14 6 -7 0.1557
14 9 -2 0.1338
5 13 12 0.1463
-4 9 16 0.1406
-13 -1 12 0.1589
-9 14 6 0.1059
4 18 0 0.1616
-7 -9 -14 0.0955
-14 -9 -4 0.1328
4 -14 -12 0.0987
-7 -16 -5 0.1397
6 -17 -3 0.1367
13 -10 -6 0.1329
15 -4 6 0.1280
9 -10 13 0.1681
0 -13 -14 0.0821
6 17 2 0.1427
-5 16 9 0.1083
9 2 16 0.1340
-15 2 -8 0.1098
-3 8 -17 0.2529

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of acetonitrile and ethyl acetate by vapour diffusion'
_exptl_crystal_size_max          0.505
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.225
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
14.9829 5.0033 -6.9895 0.0171 0.0498 1.0165
-14.9855 6.9820 -4.0016 -0.6057 -0.5311 -0.6189
13.9838 6.0018 -6.9903 -0.0137 -0.0156 0.9793
13.9830 9.0012 -1.9986 0.2059 -0.2233 0.9390
4.9916 12.9972 11.9781 0.6195 -0.7169 0.2689
-3.9979 8.9959 15.9726 0.6055 -0.6941 -0.3540
-12.9860 -1.0033 11.9811 0.2470 -0.2782 -0.9324
-8.9936 13.9842 5.9826 -0.0216 -0.9079 -0.3599
3.9917 17.9874 -0.0083 -0.0017 -0.8487 0.5143
-6.9903 -9.0028 -13.9779 -0.7871 0.5079 -0.2740
-13.9830 -9.0036 -3.9932 -0.4897 0.2910 -0.8309
3.9990 -13.9901 -11.9755 -0.3878 0.9012 0.1989
-6.9889 -15.9932 -4.9866 -0.3215 0.7596 -0.5525
5.9975 -16.9825 -2.9858 0.1053 0.9808 0.0945
12.9885 -9.9849 -5.9837 0.0994 0.7655 0.6416
14.9848 -3.9838 5.9973 0.6833 0.3572 0.6327
8.9925 -9.9800 12.9894 0.8979 0.4917 0.0840
0.0031 -12.9945 -13.9743 -0.5886 0.8138 0.0362
5.9897 16.9904 1.9900 0.1488 -0.7910 0.5693
-4.9984 15.9865 8.9784 0.2094 -0.9831 -0.1654
8.9898 2.0109 15.9792 0.9717 -0.1476 0.2293
-14.9844 1.9847 -7.9936 -0.7665 -0.2337 -0.6299
-2.9984 7.9843 -16.9816 -0.9251 -0.2564 0.2777

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36587
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.786
_diffrn_reflns_theta_min         3.413
_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 0.923
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00  13.00   1.00    5.00    --   -9.43 -38.00   0.00   95
  2  ω    -20.00  30.00   1.00    5.00    --   -9.43 -99.00 120.00   50
  3  ω    -85.00 -39.00   1.00    5.00    --   -9.43 155.00-172.97   46
  4  ω    -62.00  33.00   1.00    5.00    --   10.92 -38.00 -60.00   95
  5  ω    -20.00  51.00   1.00    5.00    --   10.92 -99.00 -90.00   71
  6  ω    -20.00  51.00   1.00    5.00    --   10.92 -99.00-150.00   71
  7  ω    -16.00  81.00   1.00    5.00    --   10.92  57.00  90.00   97
  8  ω    -20.00   5.00   1.00    5.00    --   10.92  77.00 -90.00   25
  9  ω    -20.00  51.00   1.00    5.00    --   10.92 -99.00  90.00   71
;
_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      0.0251324000
_diffrn_orient_matrix_UB_12      -0.0056526000
_diffrn_orient_matrix_UB_13      0.0473800000
_diffrn_orient_matrix_UB_21      0.0149243000
_diffrn_orient_matrix_UB_22      -0.0504987000
_diffrn_orient_matrix_UB_23      -0.0112768000
_diffrn_orient_matrix_UB_31      0.0538690000
_diffrn_orient_matrix_UB_32      0.0166304000
_diffrn_orient_matrix_UB_33      -0.0180464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4952
_reflns_number_total             5540
_reflns_odcompleteness_completeness 99.75
_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 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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         0.813
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5540
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0415
_refine_ls_restrained_S_all      1.087
_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)+(0.0234P)²+5.3958P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0955
_refine_special_details          
;
O-bound H atoms were identified from a difference Fourier map and refined as riding, with distance restraints.   One of the ethyldiethanolamine ligands was modelled with two of the ethanol arms disordered over two sites.  Appropriate displacement ellipsoid and geometric similarity restraints were used.

 
#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
410_ALERT_2_B Short Intra H...H Contact  H11A   ..  H9B     ..       1.85 Ang.

Consequence of disorder.  Atom C11 could not be reasonably split (both parts kept moving back to the same site!).

#===============================================================================
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of        C11 Check
410_ALERT_2_C Short Intra H...H Contact  H7A    ..  H11B    ..       1.95 Ang.
411_ALERT_2_C Short Inter H...H Contact  H2A    ..  H8AB    ..       2.10 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      4.367 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           8 Note
977_ALERT_2_C Check the Negative Difference Density on    H10D      -0.32 eA-3
977_ALERT_2_C Check the Negative Difference Density on    H11B      -0.36 eA-3
977_ALERT_2_C Check the Negative Difference Density on    H10B      -0.34 eA-3

All mostly a consequence of the disorder explained above.

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         14 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         10 Report
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       5.40 Why ?
171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records          2 Report
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          8 Report
187_ALERT_4_G The CIF-Embedded .res File Contains RIGU Records          4 Report
301_ALERT_3_G Main Residue  Disorder ............ Percentage =         16 Note
432_ALERT_2_G Short Inter X...Y Contact  Cl2    ..  C7A     ..       3.22 Ang.
720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          6 Note
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.13 Ratio
793_ALERT_4_G The Model has Chirality at N1      (Centro SPGR)          S Verify
860_ALERT_3_G Number of Least-Squares Restraints .............         43 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        447 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
978_ALERT_2_G Number C-C Bonds with Positive Residual Density           4 Note

Nothing significant.

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C8, C8A}
{C10, C10A}
3. Restrained distances
 O2-H2 = O4-H4
 0.84 with sigma of 0.02
 C8-C7A \\sim C8-C7
 with sigma of 0.02
 N2-C7A \\sim N2-C7
 with sigma of 0.02
 C9A-C10A \\sim C9-C10A
 with sigma of 0.02
 N2-C9A \\sim N2-C9
 with sigma of 0.02
 C8A-C7A \\sim C8-C7
 with sigma of 0.02
 O3-C8A \\sim O3-C8
 with sigma of 0.02
 O4-C10 \\sim O4-C10A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C8A)
Uanis(C10) = Uanis(C10A)
5. Rigid body (RIGU) restrains
 O3, C7A, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C9, C10A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C9A, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C9)=Sof(H9A)=Sof(H9B)=1-FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=1-FVAR(2)
 Sof(C8)=Sof(H8A)=Sof(H8B)=FVAR(2)
 Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(3)
 Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B),
 C7A(H7AA,H7AB), C8(H8A,H8B), C8A(H8AA,H8AB), C9(H9A,H9B), C9A(H9AA,H9AB),
 C10(H10A,H10B), C10A(H10C,H10D), C11(H11A,H11B)
7.b Aromatic/amide H refined with riding coordinates:
 C13(H13)
7.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C)
;
_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 0.63297(3) 0.78644(3) 0.27687(3) 0.01409(10) Uani 1 1 d . . . . .
Cr2 Cr 0.88050(3) 0.82162(3) 0.23592(3) 0.01490(10) Uani 1 1 d . . . . .
Cl1 Cl 0.52630(6) 0.67639(5) 0.36823(5) 0.02437(15) Uani 1 1 d . . . . .
Cl2 Cl 0.99055(6) 0.89409(7) 0.11688(5) 0.03174(17) Uani 1 1 d . . . . .
O1 O 0.72888(15) 0.87867(14) 0.20174(13) 0.0173(4) Uani 1 1 d . . . . .
O2 O 0.58868(16) 0.89636(15) 0.37015(14) 0.0202(4) Uani 1 1 d D . . . .
H2 H 0.638(2) 0.934(2) 0.398(2) 0.024 Uiso 1 1 d DR . . . .
O3 O 0.78438(15) 0.76396(14) 0.33838(13) 0.0169(4) Uani 1 1 d D U . . .
O4 O 0.92308(17) 0.93816(15) 0.32296(15) 0.0236(4) Uani 1 1 d D U . . .
H4 H 0.874(2) 0.963(3) 0.360(2) 0.028 Uiso 1 1 d DR . . . .
O5 O 0.66162(15) 0.67821(14) 0.17992(14) 0.0198(4) Uani 1 1 d . . . . .
O6 O 0.85072(16) 0.70263(15) 0.15064(14) 0.0215(4) Uani 1 1 d . . . . .
N1 N 0.49739(18) 0.85118(17) 0.19258(16) 0.0177(4) Uani 1 1 d . . . . .
N2 N 1.01233(19) 0.74768(18) 0.31575(16) 0.0205(5) Uani 1 1 d D . . . .
C1 C 0.5530(2) 0.9273(2) 0.1263(2) 0.0227(5) Uani 1 1 d . . . . .
H1A H 0.550889 0.994718 0.157167 0.027 Uiso 1 1 calc R . . . .
H1B H 0.509573 0.930703 0.063358 0.027 Uiso 1 1 calc R . . . .
C2 C 0.6769(2) 0.8977(2) 0.10784(19) 0.0206(5) Uani 1 1 d . . . . .
H2A H 0.679831 0.836498 0.066468 0.025 Uiso 1 1 calc R . . . .
H2B H 0.717995 0.952798 0.074134 0.025 Uiso 1 1 calc R . . . .
C3 C 0.4217(2) 0.9020(2) 0.2655(2) 0.0257(6) Uani 1 1 d . . . . .
H3A H 0.375214 0.850808 0.299858 0.031 Uiso 1 1 calc R . . . .
H3B H 0.367907 0.948466 0.231001 0.031 Uiso 1 1 calc R . . . .
C4 C 0.4934(3) 0.9600(2) 0.3389(2) 0.0294(6) Uani 1 1 d . . . . .
H4A H 0.523046 1.022558 0.308768 0.035 Uiso 1 1 calc R . . . .
H4B H 0.445920 0.978697 0.395720 0.035 Uiso 1 1 calc R . . . .
C5 C 0.4301(2) 0.7748(2) 0.1336(2) 0.0226(5) Uani 1 1 d . . . . .
H5A H 0.405648 0.720088 0.177962 0.027 Uiso 1 1 calc R . . . .
H5B H 0.482138 0.744771 0.084721 0.027 Uiso 1 1 calc R . . . .
C6 C 0.3233(2) 0.8155(2) 0.0800(2) 0.0284(6) Uani 1 1 d . . . . .
H6A H 0.346505 0.867444 0.033221 0.043 Uiso 1 1 calc GR . . . .
H6B H 0.270368 0.844857 0.127495 0.043 Uiso 1 1 calc GR . . . .
H6C H 0.284340 0.760493 0.044805 0.043 Uiso 1 1 calc GR . . . .
C7 C 0.9462(4) 0.6529(4) 0.3546(4) 0.0195(13) Uani 0.531(8) 1 d D U P A 1
H7A H 0.939726 0.602000 0.301808 0.023 Uiso 0.531(8) 1 calc R . P A 1
H7B H 0.990807 0.622584 0.409693 0.023 Uiso 0.531(8) 1 calc R . P A 1
C7A C 0.9635(5) 0.6989(6) 0.4002(5) 0.0256(16) Uani 0.469(8) 1 d D U P A 2
H7AA H 0.976039 0.742034 0.458575 0.031 Uiso 0.469(8) 1 calc R . P A 2
H7AB H 1.004015 0.634200 0.412108 0.031 Uiso 0.469(8) 1 calc R . P A 2
C8 C 0.8343(3) 0.6788(2) 0.3867(3) 0.0317(7) Uani 0.55(5) 1 d D U P A 1
H8A H 0.838332 0.692648 0.457872 0.038 Uiso 0.55(5) 1 calc R . P A 1
H8B H 0.782557 0.620156 0.376534 0.038 Uiso 0.55(5) 1 calc R . P A 1
C8A C 0.8343(3) 0.6788(2) 0.3867(3) 0.0317(7) Uani 0.45(5) 1 d D U P A 2
H8AA H 0.821755 0.617343 0.346795 0.038 Uiso 0.45(5) 1 calc R . P A 2
H8AB H 0.798001 0.668668 0.451078 0.038 Uiso 0.45(5) 1 calc R . P A 2
C9 C 1.0910(5) 0.8397(4) 0.3495(5) 0.0232(16) Uani 0.469(8) 1 d D U P A 2
H9A H 1.140846 0.818281 0.405243 0.028 Uiso 0.469(8) 1 calc R . P A 2
H9B H 1.141864 0.858979 0.294987 0.028 Uiso 0.469(8) 1 calc R . P A 2
C9A C 1.0449(5) 0.8126(4) 0.3995(4) 0.0246(14) Uani 0.531(8) 1 d D U P A 1
H9AA H 1.127007 0.800640 0.417423 0.030 Uiso 0.531(8) 1 calc R . P A 1
H9AB H 0.997556 0.794318 0.456573 0.030 Uiso 0.531(8) 1 calc R . P A 1
C10 C 1.0279(3) 0.9218(3) 0.3768(4) 0.0506(11) Uani 0.36(6) 1 d D U P A 1
H10A H 1.026237 0.960628 0.438618 0.061 Uiso 0.36(6) 1 calc R . P A 1
H10B H 1.093847 0.946448 0.338136 0.061 Uiso 0.36(6) 1 calc R . P A 1
C10A C 1.0279(3) 0.9218(3) 0.3768(4) 0.0506(11) Uani 0.64(6) 1 d D U P A 2
H10C H 1.077009 0.982462 0.370281 0.061 Uiso 0.64(6) 1 calc R . P A 2
H10D H 1.009168 0.914677 0.446888 0.061 Uiso 0.64(6) 1 calc R . P A 2
C11 C 1.0991(3) 0.6968(3) 0.2553(2) 0.0428(9) Uani 1 1 d . . . . .
H11A H 1.134361 0.748296 0.212629 0.051 Uiso 1 1 calc R . . . .
H11B H 1.057745 0.648578 0.211882 0.051 Uiso 1 1 calc R . . . .
C12 C 1.1953(2) 0.6408(2) 0.3064(2) 0.0283(6) Uani 1 1 d . . . . .
H12A H 1.247711 0.612943 0.257648 0.042 Uiso 1 1 calc GR . . . .
H12B H 1.162974 0.585851 0.345261 0.042 Uiso 1 1 calc GR . . . .
H12C H 1.238107 0.687036 0.349607 0.042 Uiso 1 1 calc GR . . . .
C13 C 0.7555(2) 0.6585(2) 0.1392(2) 0.0225(5) Uani 1 1 d . . . . .
H13 H 0.754295 0.603628 0.094506 0.027 Uiso 1 1 calc R . . . .
Cl3 Cl 0.75642(6) 1.03966(5) 0.45371(5) 0.02351(14) 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 2.2944(7) . ?
Cr1 O1 1.9546(18) . ?
Cr1 O2 2.0088(19) . ?
Cr1 O3 1.9532(18) . ?
Cr1 O5 1.9852(18) . ?
Cr1 N1 2.113(2) . ?
Cr2 Cl2 2.2930(8) . ?
Cr2 O1 1.9601(18) . ?
Cr2 O3 1.9576(18) . ?
Cr2 O4 2.007(2) . ?
Cr2 O6 1.9889(19) . ?
Cr2 N2 2.103(2) . ?
O1 C2 1.430(3) . ?
O2 H2 0.841(18) . ?
O2 C4 1.448(3) . ?
O3 C8 1.426(3) . ?
O3 C8A 1.426(3) . ?
O4 H4 0.838(18) . ?
O4 C10 1.425(4) . ?
O4 C10A 1.425(4) . ?
O5 C13 1.256(3) . ?
O6 C13 1.256(3) . ?
N1 C1 1.507(3) . ?
N1 C3 1.497(3) . ?
N1 C5 1.504(3) . ?
N2 C7 1.570(5) . ?
N2 C7A 1.446(6) . ?
N2 C9 1.587(6) . ?
N2 C9A 1.476(5) . ?
N2 C11 1.474(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.512(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.502(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.525(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.417(6) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C7A C8A 1.527(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10A 1.366(7) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C9A C10 1.494(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10A H10C 0.9900 . ?
C10A H10D 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.502(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 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
O1 Cr1 Cl1 177.91(6) . . ?
O1 Cr1 O2 91.79(8) . . ?
O1 Cr1 O5 90.03(8) . . ?
O1 Cr1 N1 83.24(8) . . ?
O2 Cr1 Cl1 88.41(6) . . ?
O2 Cr1 N1 81.68(8) . . ?
O3 Cr1 Cl1 98.96(6) . . ?
O3 Cr1 O1 78.96(7) . . ?
O3 Cr1 O2 94.29(8) . . ?
O3 Cr1 O5 91.01(8) . . ?
O3 Cr1 N1 161.62(8) . . ?
O5 Cr1 Cl1 89.96(6) . . ?
O5 Cr1 O2 174.64(8) . . ?
O5 Cr1 N1 93.53(8) . . ?
N1 Cr1 Cl1 98.85(6) . . ?
O1 Cr2 Cl2 100.05(6) . . ?
O1 Cr2 O4 93.06(8) . . ?
O1 Cr2 O6 91.24(8) . . ?
O1 Cr2 N2 160.45(8) . . ?
O3 Cr2 Cl2 178.18(6) . . ?
O3 Cr2 O1 78.72(7) . . ?
O3 Cr2 O4 90.84(8) . . ?
O3 Cr2 O6 90.75(8) . . ?
O3 Cr2 N2 82.12(8) . . ?
O4 Cr2 Cl2 87.87(7) . . ?
O4 Cr2 N2 83.32(9) . . ?
O6 Cr2 Cl2 90.62(6) . . ?
O6 Cr2 O4 175.64(8) . . ?
O6 Cr2 N2 92.88(9) . . ?
N2 Cr2 Cl2 99.01(7) . . ?
Cr1 O1 Cr2 98.44(8) . . ?
C2 O1 Cr1 110.33(15) . . ?
C2 O1 Cr2 130.03(16) . . ?
Cr1 O2 H2 123(2) . . ?
C4 O2 Cr1 115.95(16) . . ?
C4 O2 H2 107(2) . . ?
Cr1 O3 Cr2 98.57(8) . . ?
C8 O3 Cr1 132.33(17) . . ?
C8 O3 Cr2 114.21(17) . . ?
C8A O3 Cr1 132.33(17) . . ?
C8A O3 Cr2 114.21(17) . . ?
Cr2 O4 H4 120(2) . . ?
C10 O4 Cr2 112.7(2) . . ?
C10 O4 H4 109(2) . . ?
C10A O4 Cr2 112.7(2) . . ?
C10A O4 H4 109(2) . . ?
C13 O5 Cr1 126.97(18) . . ?
C13 O6 Cr2 125.91(17) . . ?
C1 N1 Cr1 106.18(15) . . ?
C3 N1 Cr1 104.95(16) . . ?
C3 N1 C1 111.0(2) . . ?
C3 N1 C5 110.9(2) . . ?
C5 N1 Cr1 113.02(16) . . ?
C5 N1 C1 110.6(2) . . ?
C7 N2 Cr2 101.3(2) . . ?
C7A N2 Cr2 109.4(3) . . ?
C7A N2 C9 110.1(4) . . ?
C7A N2 C11 121.4(4) . . ?
C9 N2 Cr2 101.5(3) . . ?
C9A N2 Cr2 107.6(3) . . ?
C9A N2 C7 109.0(3) . . ?
C11 N2 Cr2 114.70(18) . . ?
C11 N2 C7 99.4(3) . . ?
C11 N2 C9 97.0(3) . . ?
C11 N2 C9A 122.3(3) . . ?
N1 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
N1 C1 C2 110.0(2) . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
O1 C2 C1 106.4(2) . . ?
O1 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.6 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 C4 110.6(2) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
O2 C4 C3 107.9(2) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
N1 C5 H5A 108.5 . . ?
N1 C5 H5B 108.5 . . ?
N1 C5 C6 115.2(2) . . ?
H5A C5 H5B 107.5 . . ?
C6 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 N2 111.3(4) . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
N2 C7A H7AA 109.2 . . ?
N2 C7A H7AB 109.2 . . ?
N2 C7A C8A 112.1(4) . . ?
H7AA C7A H7AB 107.9 . . ?
C8A C7A H7AA 109.2 . . ?
C8A C7A H7AB 109.2 . . ?
O3 C8 H8A 108.6 . . ?
O3 C8 H8B 108.6 . . ?
C7 C8 O3 114.5(3) . . ?
C7 C8 H8A 108.6 . . ?
C7 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
O3 C8A C7A 107.8(3) . . ?
O3 C8A H8AA 110.1 . . ?
O3 C8A H8AB 110.1 . . ?
C7A C8A H8AA 110.1 . . ?
C7A C8A H8AB 110.1 . . ?
H8AA C8A H8AB 108.5 . . ?
N2 C9 H9A 109.0 . . ?
N2 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C10A C9 N2 112.8(4) . . ?
C10A C9 H9A 109.0 . . ?
C10A C9 H9B 109.0 . . ?
N2 C9A H9AA 109.2 . . ?
N2 C9A H9AB 109.2 . . ?
N2 C9A C10 112.0(4) . . ?
H9AA C9A H9AB 107.9 . . ?
C10 C9A H9AA 109.2 . . ?
C10 C9A H9AB 109.2 . . ?
O4 C10 C9A 111.3(3) . . ?
O4 C10 H10A 109.4 . . ?
O4 C10 H10B 109.4 . . ?
C9A C10 H10A 109.4 . . ?
C9A C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
O4 C10A H10C 108.3 . . ?
O4 C10A H10D 108.3 . . ?
C9 C10A O4 115.8(4) . . ?
C9 C10A H10C 108.3 . . ?
C9 C10A H10D 108.3 . . ?
H10C C10A H10D 107.4 . . ?
N2 C11 H11A 107.8 . . ?
N2 C11 H11B 107.8 . . ?
N2 C11 C12 118.2(3) . . ?
H11A C11 H11B 107.1 . . ?
C12 C11 H11A 107.8 . . ?
C12 C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 H13 116.2 . . ?
O6 C13 O5 127.7(2) . . ?
O6 C13 H13 116.2 . . ?

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
O2 H2 Cl3 0.841(18) 2.098(19) 2.935(2) 173(3) .
O4 H4 Cl3 0.838(18) 2.138(19) 2.972(2) 174(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 C2 C1 50.6(2) . . . . ?
Cr1 O2 C4 C3 23.3(3) . . . . ?
Cr1 O3 C8 C7 131.2(3) . . . . ?
Cr1 O3 C8A C7A 168.2(3) . . . . ?
Cr1 O5 C13 O6 -0.2(4) . . . . ?
Cr1 N1 C1 C2 26.5(3) . . . . ?
Cr1 N1 C3 C4 44.7(3) . . . . ?
Cr1 N1 C5 C6 173.67(19) . . . . ?
Cr2 O1 C2 C1 171.62(16) . . . . ?
Cr2 O3 C8 C7 2.1(4) . . . . ?
Cr2 O3 C8A C7A 39.1(4) . . . . ?
Cr2 O4 C10 C9A -31.3(5) . . . . ?
Cr2 O4 C10A C9 10.3(5) . . . . ?
Cr2 O6 C13 O5 -1.7(4) . . . . ?
Cr2 N2 C7 C8 -41.6(4) . . . . ?
Cr2 N2 C7A C8A 22.5(6) . . . . ?
Cr2 N2 C9 C10A 39.9(5) . . . . ?
Cr2 N2 C9A C10 -30.0(5) . . . . ?
Cr2 N2 C11 C12 -179.1(3) . . . . ?
N1 C1 C2 O1 -50.3(3) . . . . ?
N1 C3 C4 O2 -45.4(3) . . . . ?
N2 C7 C8 O3 28.3(5) . . . . ?
N2 C7A C8A O3 -39.7(6) . . . . ?
N2 C9 C10A O4 -35.1(7) . . . . ?
N2 C9A C10 O4 41.2(6) . . . . ?
C1 N1 C3 C4 -69.5(3) . . . . ?
C1 N1 C5 C6 -67.4(3) . . . . ?
C3 N1 C1 C2 140.0(2) . . . . ?
C3 N1 C5 C6 56.1(3) . . . . ?
C5 N1 C1 C2 -96.5(3) . . . . ?
C5 N1 C3 C4 167.1(2) . . . . ?
C7 N2 C9A C10 -139.1(4) . . . . ?
C7 N2 C11 C12 -72.0(4) . . . . ?
C7A N2 C9 C10A -75.9(6) . . . . ?
C7A N2 C11 C12 -43.9(6) . . . . ?
C9 N2 C7A C8A 133.2(5) . . . . ?
C9 N2 C11 C12 74.8(4) . . . . ?
C9A N2 C7 C8 71.7(5) . . . . ?
C9A N2 C11 C12 47.7(5) . . . . ?
C11 N2 C7 C8 -159.3(4) . . . . ?
C11 N2 C7A C8A -114.7(5) . . . . ?
C11 N2 C9 C10A 156.9(5) . . . . ?
C11 N2 C9A C10 106.0(5) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-11
_olex2_date_sample_submission    2016-11-11
_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 L35o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.766
_oxdiff_exptl_absorpt_empirical_full_min 0.714
####################################################################### 
# 
# 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 1579644'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
# local name eb16280
_audit_creation_date             2016-12-06
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H33 Cl2 Cr2 N2 O6, Cl'
_chemical_formula_sum            'C15 H33 Cl3 Cr2 N2 O6'
_chemical_formula_weight         547.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr2 Cl '
_chemical_oxdiff_usercomment     '@ 120 K L144'
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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.0747(4)
_cell_length_b                   10.3531(2)
_cell_length_c                   31.3324(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4565.6(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    12842
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      30.9410
_cell_measurement_theta_min      3.4760
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
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            'pale green'
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2272
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0131
0 0 -1 0.0131
8 -13 4 0.2103
-11 -12 1 0.2164
-20 1 -3 0.2170
11 12 -1 0.1485
20 0 3 0.2077
-1 5 -1 0.2065

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from acetonitrile by hydrothermal bomb'
_exptl_crystal_size_max          0.525
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.026
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
0.0002 0.0007 1.0002 0.0224 0.0029 0.0019
-0.0002 -0.0007 -1.0002 -0.0224 -0.0029 -0.0019
7.6309 -13.4036 4.1561 0.0440 -0.2445 0.9687
-10.5894 -12.3419 1.3184 -0.1201 0.6396 0.7592
-19.7752 0.7177 -2.9803 -0.1790 0.9638 -0.1977
11.2334 12.0318 -1.1557 0.1254 -0.6682 -0.7333
19.7951 -0.3752 2.9047 0.1798 -0.9681 0.1746
-1.0004 4.9968 -1.0012 0.0068 0.0015 -0.3467

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            48743
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.223
_diffrn_reflns_theta_min         2.767
_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 0.9979
_diffrn_measured_fraction_theta_max 0.9246
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -100.00  73.00   1.00   10.00    --  -13.24   0.00 150.00  173
  2  ω      1.00  27.00   1.00   10.00    --  -13.24 -99.00 -60.00   26
  3  ω    -77.00 -50.00   1.00   10.00    --  -13.24 147.00  32.00   27
  4  ω    -83.00  13.00   1.00   10.00    --  -13.24 -57.00  60.00   96
  5  ω     14.00  41.00   1.00   10.00    --   14.65 -57.00 120.00   27
  6  ω     34.00  61.00   1.00   10.00    --   14.65-178.00-180.00   27
;
_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      0.0059351000
_diffrn_orient_matrix_UB_12      0.0070304000
_diffrn_orient_matrix_UB_13      0.0223654000
_diffrn_orient_matrix_UB_21      -0.0495106000
_diffrn_orient_matrix_UB_22      -0.0090286000
_diffrn_orient_matrix_UB_23      0.0029602000
_diffrn_orient_matrix_UB_31      0.0072585000
_diffrn_orient_matrix_UB_32      -0.0675406000
_diffrn_orient_matrix_UB_33      0.0019196000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5507
_reflns_number_total             6888
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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         0.520
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         6888
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0506
_refine_ls_restrained_S_all      1.110
_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)+(0.0261P)²+4.7343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0990
_refine_special_details          
;
O-bound H atoms were identified from 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
 
906_ALERT_3_C Large K value in the Analysis of Variance ......      7.246 Check

Not significant

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          4 Note
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
793_ALERT_4_G The Model has Chirality at N1      (Centro SPGR)          S Verify
793_ALERT_4_G The Model has Chirality at N2      (Centro SPGR)          S Verify
860_ALERT_3_G Number of Least-Squares Restraints .............          2 Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           4 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        507 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
952_ALERT_5_G Calculated (ThMax) and CIF-Reported Lmax Differ           2 Units
958_ALERT_1_G Calculated (ThMax) and Actual (FCF) Lmax Differ           2 Units
978_ALERT_2_G Number C-C Bonds with Positive Residual Density           3 Note

Not significant
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4 = O2-H2
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C)
;
_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 0.51073(3) 0.67917(4) 0.13741(2) 0.00965(9) Uani 1 1 d . . . . .
Cr2 Cr 0.47862(3) 0.96057(4) 0.14480(2) 0.00997(9) Uani 1 1 d . . . . .
Cl1 Cl 0.62914(5) 0.53517(6) 0.15395(2) 0.01651(13) Uani 1 1 d . . . . .
Cl2 Cl 0.39807(5) 1.11989(6) 0.10767(2) 0.01831(14) Uani 1 1 d . . . . .
Cl3 Cl 0.27881(5) 0.75389(6) 0.22171(2) 0.02074(15) Uani 1 1 d . . . . .
O1 O 0.41274(12) 0.80621(15) 0.12423(6) 0.0123(4) Uani 1 1 d . . . . .
O2 O 0.42937(13) 0.59700(17) 0.18279(6) 0.0161(4) Uani 1 1 d D . . . .
H2 H 0.3869(18) 0.639(3) 0.1939(9) 0.019 Uiso 1 1 d DR . . . .
O3 O 0.54924(12) 0.82249(15) 0.17368(5) 0.0105(3) Uani 1 1 d . . . . .
O4 O 0.38838(13) 0.97979(17) 0.19354(6) 0.0157(4) Uani 1 1 d D . . . .
H4 H 0.357(2) 0.915(2) 0.2018(9) 0.019 Uiso 1 1 d DR . . . .
O5 O 0.58486(13) 0.74110(16) 0.08824(5) 0.0141(4) Uani 1 1 d . . . . .
O6 O 0.57144(13) 0.95553(16) 0.09721(5) 0.0134(4) Uani 1 1 d . . . . .
N1 N 0.42683(16) 0.56317(19) 0.09661(7) 0.0149(4) Uani 1 1 d . . . . .
N2 N 0.56362(15) 1.07880(19) 0.18331(7) 0.0140(4) Uani 1 1 d . . . . .
C1 C 0.3796(2) 0.6582(3) 0.06770(9) 0.0229(6) Uani 1 1 d . . . . .
H1A H 0.325419 0.616268 0.053049 0.027 Uiso 1 1 calc R . . . .
H1B H 0.425201 0.687517 0.045698 0.027 Uiso 1 1 calc R . . . .
C2 C 0.3442(2) 0.7736(3) 0.09293(9) 0.0214(6) Uani 1 1 d . . . . .
H2A H 0.333786 0.847794 0.073561 0.026 Uiso 1 1 calc R . . . .
H2B H 0.283026 0.752335 0.106861 0.026 Uiso 1 1 calc R . . . .
C3 C 0.3541(2) 0.4948(3) 0.12369(10) 0.0249(6) Uani 1 1 d . . . . .
H3A H 0.295177 0.546923 0.125067 0.030 Uiso 1 1 calc R . . . .
H3B H 0.338340 0.410197 0.110789 0.030 Uiso 1 1 calc R . . . .
C4 C 0.3926(2) 0.4753(3) 0.16760(10) 0.0242(6) Uani 1 1 d . . . . .
H4A H 0.341678 0.444277 0.186842 0.029 Uiso 1 1 calc R . . . .
H4B H 0.443841 0.409807 0.167085 0.029 Uiso 1 1 calc R . . . .
C5 C 0.4812(2) 0.4692(3) 0.07084(10) 0.0253(6) Uani 1 1 d . . . . .
H5A H 0.534111 0.513422 0.056702 0.038 Uiso 1 1 calc GR . . . .
H5B H 0.439420 0.430868 0.049261 0.038 Uiso 1 1 calc GR . . . .
H5C H 0.506063 0.401119 0.089460 0.038 Uiso 1 1 calc GR . . . .
C6 C 0.63023(19) 0.9912(2) 0.20828(8) 0.0166(5) Uani 1 1 d . . . . .
H6A H 0.692579 1.034120 0.211893 0.020 Uiso 1 1 calc R . . . .
H6B H 0.603475 0.974343 0.236966 0.020 Uiso 1 1 calc R . . . .
C7 C 0.64305(18) 0.8647(2) 0.18454(8) 0.0134(5) Uani 1 1 d . . . . .
H7A H 0.681654 0.877767 0.158485 0.016 Uiso 1 1 calc R . . . .
H7B H 0.675070 0.800202 0.202898 0.016 Uiso 1 1 calc R . . . .
C8 C 0.49535(19) 1.1450(2) 0.21266(9) 0.0175(5) Uani 1 1 d . . . . .
H8A H 0.461317 1.213909 0.196988 0.021 Uiso 1 1 calc R . . . .
H8B H 0.530596 1.185455 0.236508 0.021 Uiso 1 1 calc R . . . .
C9 C 0.4249(2) 1.0491(3) 0.23005(8) 0.0195(6) Uani 1 1 d . . . . .
H9A H 0.456268 0.989038 0.250186 0.023 Uiso 1 1 calc R . . . .
H9B H 0.372822 1.094187 0.245216 0.023 Uiso 1 1 calc R . . . .
C10 C 0.6199(2) 1.1761(2) 0.15959(9) 0.0202(6) Uani 1 1 d . . . . .
H10A H 0.668049 1.132361 0.142241 0.030 Uiso 1 1 calc GR . . . .
H10B H 0.651167 1.234363 0.179861 0.030 Uiso 1 1 calc GR . . . .
H10C H 0.577683 1.226099 0.140981 0.030 Uiso 1 1 calc GR . . . .
C11 C 0.60107(18) 0.8568(2) 0.07758(8) 0.0128(5) Uani 1 1 d . . . . .
C12 C 0.6645(2) 0.8772(3) 0.03873(8) 0.0173(5) Uani 1 1 d . . . . .
C13 C 0.6450(2) 0.7720(3) 0.00562(9) 0.0235(6) Uani 1 1 d . . . . .
H13A H 0.658092 0.687104 0.018149 0.035 Uiso 1 1 calc GR . . . .
H13B H 0.686024 0.785289 -0.019251 0.035 Uiso 1 1 calc GR . . . .
H13C H 0.578262 0.776125 -0.003241 0.035 Uiso 1 1 calc GR . . . .
C14 C 0.7668(2) 0.8658(4) 0.05518(10) 0.0361(8) Uani 1 1 d . . . . .
H14A H 0.779561 0.935728 0.075469 0.054 Uiso 1 1 calc GR . . . .
H14B H 0.811066 0.872078 0.031128 0.054 Uiso 1 1 calc GR . . . .
H14C H 0.775111 0.782347 0.069453 0.054 Uiso 1 1 calc GR . . . .
C15 C 0.6478(3) 1.0096(3) 0.01895(11) 0.0368(8) Uani 1 1 d . . . . .
H15A H 0.581989 1.015699 0.008984 0.055 Uiso 1 1 calc GR . . . .
H15B H 0.691112 1.021621 -0.005232 0.055 Uiso 1 1 calc GR . . . .
H15C H 0.659690 1.076699 0.040356 0.055 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 2.2954(7) . ?
Cr1 O1 1.9499(17) . ?
Cr1 O2 2.0141(18) . ?
Cr1 O3 1.9462(16) . ?
Cr1 O5 1.9679(18) . ?
Cr1 N1 2.114(2) . ?
Cr2 Cl2 2.3150(7) . ?
Cr2 O1 1.9569(17) . ?
Cr2 O3 1.9623(16) . ?
Cr2 O4 1.9961(18) . ?
Cr2 O6 1.9831(18) . ?
Cr2 N2 2.094(2) . ?
O1 C2 1.416(3) . ?
O2 H2 0.819(17) . ?
O2 C4 1.443(3) . ?
O3 C7 1.432(3) . ?
O4 H4 0.845(17) . ?
O4 C9 1.445(3) . ?
O5 C11 1.264(3) . ?
O6 C11 1.264(3) . ?
N1 C1 1.494(3) . ?
N1 C3 1.506(4) . ?
N1 C5 1.477(3) . ?
N2 C6 1.521(3) . ?
N2 C8 1.496(3) . ?
N2 C10 1.482(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.516(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.493(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.517(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.505(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.524(3) . ?
C12 C13 1.529(4) . ?
C12 C14 1.534(4) . ?
C12 C15 1.522(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 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
O1 Cr1 Cl1 178.04(6) . . ?
O1 Cr1 O2 91.85(8) . . ?
O1 Cr1 O5 89.40(7) . . ?
O1 Cr1 N1 81.96(8) . . ?
O2 Cr1 Cl1 88.80(6) . . ?
O2 Cr1 N1 82.50(8) . . ?
O3 Cr1 Cl1 99.27(5) . . ?
O3 Cr1 O1 78.84(7) . . ?
O3 Cr1 O2 93.90(7) . . ?
O3 Cr1 O5 93.50(7) . . ?
O3 Cr1 N1 160.34(8) . . ?
O5 Cr1 Cl1 90.19(6) . . ?
O5 Cr1 O2 172.59(8) . . ?
O5 Cr1 N1 90.45(8) . . ?
N1 Cr1 Cl1 99.97(6) . . ?
O1 Cr2 Cl2 100.62(5) . . ?
O1 Cr2 O3 78.29(7) . . ?
O1 Cr2 O4 91.83(7) . . ?
O1 Cr2 O6 92.46(7) . . ?
O1 Cr2 N2 159.69(8) . . ?
O3 Cr2 Cl2 177.28(6) . . ?
O3 Cr2 O4 92.41(7) . . ?
O3 Cr2 O6 89.65(7) . . ?
O3 Cr2 N2 82.57(8) . . ?
O4 Cr2 Cl2 90.11(6) . . ?
O4 Cr2 N2 82.21(8) . . ?
O6 Cr2 Cl2 87.91(5) . . ?
O6 Cr2 O4 175.54(7) . . ?
O6 Cr2 N2 94.15(8) . . ?
N2 Cr2 Cl2 98.79(6) . . ?
Cr1 O1 Cr2 98.40(8) . . ?
C2 O1 Cr1 117.87(15) . . ?
C2 O1 Cr2 138.20(15) . . ?
Cr1 O2 H2 119(2) . . ?
C4 O2 Cr1 109.88(16) . . ?
C4 O2 H2 110(2) . . ?
Cr1 O3 Cr2 98.33(7) . . ?
C7 O3 Cr1 128.94(15) . . ?
C7 O3 Cr2 110.75(14) . . ?
Cr2 O4 H4 119(2) . . ?
C9 O4 Cr2 115.41(16) . . ?
C9 O4 H4 110(2) . . ?
C11 O5 Cr1 127.68(16) . . ?
C11 O6 Cr2 127.21(16) . . ?
C1 N1 Cr1 103.95(15) . . ?
C1 N1 C3 110.4(2) . . ?
C3 N1 Cr1 107.81(16) . . ?
C5 N1 Cr1 114.53(17) . . ?
C5 N1 C1 109.4(2) . . ?
C5 N1 C3 110.5(2) . . ?
C6 N2 Cr2 107.47(14) . . ?
C8 N2 Cr2 104.77(16) . . ?
C8 N2 C6 110.6(2) . . ?
C10 N2 Cr2 114.45(17) . . ?
C10 N2 C6 109.5(2) . . ?
C10 N2 C8 109.9(2) . . ?
N1 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
N1 C1 C2 110.4(2) . . ?
H1A C1 H1B 108.1 . . ?
C2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
O1 C2 C1 109.0(2) . . ?
O1 C2 H2A 109.9 . . ?
O1 C2 H2B 109.9 . . ?
C1 C2 H2A 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
N1 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 N1 109.6(2) . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
O2 C4 C3 108.4(2) . . ?
O2 C4 H4A 110.0 . . ?
O2 C4 H4B 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C7 C6 N2 109.6(2) . . ?
C7 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
O3 C7 C6 105.7(2) . . ?
O3 C7 H7A 110.6 . . ?
O3 C7 H7B 110.6 . . ?
C6 C7 H7A 110.6 . . ?
C6 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
N2 C8 H8A 109.6 . . ?
N2 C8 H8B 109.6 . . ?
N2 C8 C9 110.1(2) . . ?
H8A C8 H8B 108.1 . . ?
C9 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
O4 C9 C8 106.0(2) . . ?
O4 C9 H9A 110.5 . . ?
O4 C9 H9B 110.5 . . ?
C8 C9 H9A 110.5 . . ?
C8 C9 H9B 110.5 . . ?
H9A C9 H9B 108.7 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 C12 116.6(2) . . ?
O6 C11 O5 125.3(2) . . ?
O6 C11 C12 118.0(2) . . ?
C11 C12 C13 109.7(2) . . ?
C11 C12 C14 105.7(2) . . ?
C13 C12 C14 110.0(2) . . ?
C15 C12 C11 111.1(2) . . ?
C15 C12 C13 109.7(2) . . ?
C15 C12 C14 110.5(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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 C2 C1 -15.6(3) . . . . ?
Cr1 O2 C4 C3 -47.0(3) . . . . ?
Cr1 O3 C7 C6 171.98(15) . . . . ?
Cr1 O5 C11 O6 -0.1(4) . . . . ?
Cr1 O5 C11 C12 177.61(16) . . . . ?
Cr1 N1 C1 C2 -43.2(3) . . . . ?
Cr1 N1 C3 C4 -28.8(3) . . . . ?
Cr2 O1 C2 C1 131.4(2) . . . . ?
Cr2 O3 C7 C6 51.6(2) . . . . ?
Cr2 O4 C9 C8 30.5(2) . . . . ?
Cr2 O6 C11 O5 -8.8(4) . . . . ?
Cr2 O6 C11 C12 173.47(16) . . . . ?
Cr2 N2 C6 C7 24.1(2) . . . . ?
Cr2 N2 C8 C9 45.1(2) . . . . ?
O5 C11 C12 C13 36.2(3) . . . . ?
O5 C11 C12 C14 -82.4(3) . . . . ?
O5 C11 C12 C15 157.7(3) . . . . ?
O6 C11 C12 C13 -145.9(2) . . . . ?
O6 C11 C12 C14 95.5(3) . . . . ?
O6 C11 C12 C15 -24.4(3) . . . . ?
N1 C1 C2 O1 39.9(3) . . . . ?
N1 C3 C4 O2 50.0(3) . . . . ?
N2 C6 C7 O3 -48.6(3) . . . . ?
N2 C8 C9 O4 -50.0(3) . . . . ?
C1 N1 C3 C4 -141.7(2) . . . . ?
C3 N1 C1 C2 72.2(3) . . . . ?
C5 N1 C1 C2 -165.9(2) . . . . ?
C5 N1 C3 C4 97.1(3) . . . . ?
C6 N2 C8 C9 -70.4(3) . . . . ?
C8 N2 C6 C7 138.0(2) . . . . ?
C10 N2 C6 C7 -100.7(2) . . . . ?
C10 N2 C8 C9 168.5(2) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_date_sample_data_collection 2016-12-01
_olex2_date_sample_submission    2016-11-24
_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 L144
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.737
####################################################################### 
# 
# 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 1579647'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
# local name eb17079b
_audit_creation_date             2017-06-08
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H27 Cl4 Cr2 N2 O6, Cl'
_chemical_formula_sum            'C17 H27 Cl5 Cr2 N2 O6'
_chemical_formula_weight         636.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C17 H27 Cl5 Cr2 N2 O6'
_chemical_oxdiff_usercomment     '@ 120 K 900o'
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                   10.2393(2)
_cell_length_b                   14.2193(3)
_cell_length_c                   18.1746(4)
_cell_angle_alpha                76.834(2)
_cell_angle_beta                 81.3824(19)
_cell_angle_gamma                89.2989(19)
_cell_volume                     2546.84(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    20339
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.7860
_cell_measurement_theta_min      4.4690
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.174
_exptl_absorpt_correction_T_max  0.47332
_exptl_absorpt_correction_T_min  0.42180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 9 6 0.0295
-1 -9 -6 0.0295
6 1 7 0.1163
-6 -1 -7 0.1163
0 4 -9 0.0147
0 -4 9 0.0147

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of methanol and acetonitrile by hydrothermal bomb'
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.029
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
0.9986 8.9932 6.0003 0.1537 1.0100 -0.0359
-0.9986 -8.9932 -6.0003 -0.1537 -1.0100 0.0359
5.9938 0.9931 7.0066 0.0883 0.3715 0.9396
-5.9938 -0.9931 -7.0066 -0.0883 -0.3715 -0.9396
0.0066 3.9981 -8.9949 0.8709 0.0228 -0.4773
-0.0066 -3.9981 8.9949 -0.8709 -0.0228 0.4773

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51940
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.399
_diffrn_reflns_theta_min         3.193
_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 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -127.00 -34.00   1.00    5.00    --  -41.67 178.00  30.00   93
  2  ω   -112.00 -15.00   1.00    5.00    --  -41.67 -57.00 -90.00   97
  3  ω    -68.00  28.00   1.00    5.00    --  -41.67  57.00  60.00   96
  4  ω     57.00 128.00   1.00    5.00    --   41.67 178.00 -60.00   71
  5  ω     10.00 116.00   1.00    5.00    --   41.67  77.00-180.00  106
  6  ω     87.00 178.00   1.00   20.00    --  111.00  45.00 120.00   91
  7  ω     80.00 178.00   1.00   20.00    --  111.00  77.00  60.00   98
  8  ω     87.00 178.00   1.00   20.00    --  111.00  30.00-150.00   91
  9  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00 -30.00  105
 10  ω     39.00 121.00   1.00   20.00    --  111.00-125.00-180.00   82
 11  ω     80.00 178.00   1.00   20.00    --  111.00  74.00 141.76   98
 12  ω     39.00 121.00   1.00   20.00    --  111.00-125.00   0.00   82
 13  ω     41.00 139.00   1.00   20.00    --  111.00 -61.00  90.00   98
 14  ω     30.00 109.00   1.00   20.00    --  111.00 -94.00  60.00   79
 15  ω     30.00 109.00   1.00   20.00    --  111.00 -94.00 -30.00   79
 16  ω     37.00 142.00   1.00   20.00    --  111.00 -77.00-180.00  105
 17  ω     87.00 178.00   1.00   20.00    --  111.00  30.00 -90.00   91
 18  ω     39.00 121.00   1.00   20.00    --  111.00-125.00  30.00   82
 19  ω     94.00 178.00   1.00   20.00    --  111.00 125.00 120.00   84
 20  ω     40.00 135.00   1.00   20.00    --  111.00 -45.00-180.00   95
 21  ω     39.00 121.00   1.00   20.00    --  111.00-125.00 150.00   82
 22  ω     39.00 121.00   1.00   20.00    --  111.00-125.00-120.00   82
 23  ω     87.00 178.00   1.00   20.00    --  111.00  45.00 150.00   91
 24  ω     39.00 121.00   1.00   20.00    --  111.00-125.00  60.00   82
 25  ω     40.00 135.00   1.00   20.00    --  111.00 -45.00 150.00   95
 26  ω     39.00 121.00   1.00   20.00    --  111.00-125.00 -60.00   82
 27  ω     94.00 178.00   1.00   20.00    --  111.00 125.00 150.00   84
 28  ω   -116.00 -10.00   1.00    5.00    --  -41.67 -77.00   0.00  106
 29  ω   -112.00 -15.00   1.00    5.00    --  -41.67 -57.00  30.00   97
 30  ω   -114.00 -19.00   1.00    5.00    --  -41.67 -38.00  90.00   95
 31  ω   -116.00 -10.00   1.00    5.00    --  -41.67 -77.00-120.00  106
 32  ω     57.00 128.00   1.00    5.00    --   41.67 178.00  30.00   71
 33  ω     85.00 178.00   1.00   20.00    --  111.00  52.00 -53.61   93
 34  ω     87.00 178.00   1.00   20.00    --  111.00  30.00   0.00   91
 35  ω     83.00 137.00   1.00   20.00    --  111.00  61.00-150.00   54
 36  ω     87.00 178.00   1.00   20.00    --  111.00  45.00  30.00   91
;
_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      0.0899546000
_diffrn_orient_matrix_UB_12      0.0552724000
_diffrn_orient_matrix_UB_13      -0.0721910000
_diffrn_orient_matrix_UB_21      0.0049773000
_diffrn_orient_matrix_UB_22      0.0874991000
_diffrn_orient_matrix_UB_23      0.0363563000
_diffrn_orient_matrix_UB_31      0.1226883000
_diffrn_orient_matrix_UB_32      -0.0409352000
_diffrn_orient_matrix_UB_33      0.0349540000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_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          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9114
_reflns_number_total             10528
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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         1.591
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         10528
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0560
_refine_ls_restrained_S_all      1.040
_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)+(0.1006P)²+1.3702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1546
_refine_special_details          
;
O-bound H atoms were identified from a difference Fourier map and refined as riding, with distance restraints.

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
213_ALERT_2_C Atom Cl3             has ADP max/min Ratio .....        3.1 prolat
220_ALERT_2_C Non-Solvent Resd 1  Cl   Ueq(max)/Ueq(min) Range        3.3 Ratio
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.193 Check
971_ALERT_2_C Check Calcd Residual Density  1.18A From     Cl3       1.51 eA-3
978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note

Not significant

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          8 Note
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.10 Report
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          1 Report
434_ALERT_2_G Short Inter HL..HL Contact Cl54   ..  Cl54    ..       3.21 Ang.
790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          4 Note
              Cl

Chosen to demonstrate O-H...Cl interaction

793_ALERT_4_G The Model has Chirality at N1      (Centro SPGR)          S Verify
793_ALERT_4_G The Model has Chirality at N2      (Centro SPGR)          S Verify
793_ALERT_4_G The Model has Chirality at N51     (Centro SPGR)          R Verify
793_ALERT_4_G The Model has Chirality at N52     (Centro SPGR)          R Verify
860_ALERT_3_G Number of Least-Squares Restraints .............          4 Note
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           1 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        137 Note
933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          2 Note

Not significant

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2 = O4-H4 = O52-H52 = O54-H54
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C31(H31A,H31B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
 C54(H54A,H54B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C16(H16), C63(H63), C65(H65), C67(H67)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C55(H55A,H55B,H55C), C60(H60A,H60B,H60C)
;
_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 -0.11384(5) 0.50447(4) 0.79733(3) 0.02078(13) Uani 1 1 d . . . . .
Cr2 Cr 0.17557(5) 0.50540(4) 0.79532(3) 0.01924(13) Uani 1 1 d . . . . .
Cl1 Cl -0.25793(9) 0.44892(8) 0.73062(6) 0.0354(2) Uani 1 1 d . . . . .
Cl2 Cl 0.33426(8) 0.59610(6) 0.82583(5) 0.02923(18) Uani 1 1 d . . . . .
Cl3 Cl -0.14863(19) 0.87020(13) 0.46218(13) 0.0976(8) Uani 1 1 d . . . . .
Cl4 Cl 0.35565(11) 0.91875(7) 0.49662(5) 0.0398(2) Uani 1 1 d . . . . .
O1 O 0.0179(2) 0.54895(17) 0.85082(14) 0.0233(5) Uani 1 1 d . . . . .
O2 O -0.1869(2) 0.40435(18) 0.89015(15) 0.0265(5) Uani 1 1 d D . . . .
H2 H -0.136(4) 0.368(3) 0.913(3) 0.032 Uiso 1 1 d DR . . . .
O3 O 0.0391(2) 0.42838(17) 0.77018(14) 0.0228(5) Uani 1 1 d . . . . .
O4 O 0.2092(3) 0.39921(18) 0.88349(14) 0.0263(5) Uani 1 1 d D . . . .
H4 H 0.143(3) 0.363(3) 0.902(3) 0.032 Uiso 1 1 d DR . . . .
O5 O -0.0577(2) 0.61141(19) 0.70666(15) 0.0271(5) Uani 1 1 d . . . . .
O6 O 0.1631(2) 0.60855(17) 0.70238(14) 0.0256(5) Uani 1 1 d . . . . .
N1 N -0.2382(3) 0.5935(2) 0.85287(18) 0.0249(6) Uani 1 1 d . . . . .
N2 N 0.2970(3) 0.4244(2) 0.73095(17) 0.0254(6) Uani 1 1 d . . . . .
C1 C -0.1566(4) 0.6387(3) 0.8989(2) 0.0286(7) Uani 1 1 d . . . . .
H1A H -0.167276 0.599956 0.952183 0.034 Uiso 1 1 calc R . . . .
H1B H -0.187527 0.704677 0.899853 0.034 Uiso 1 1 calc R . . . .
C2 C -0.0125(4) 0.6432(3) 0.8640(2) 0.0279(7) Uani 1 1 d . . . . .
H2A H 0.002640 0.692657 0.815301 0.033 Uiso 1 1 calc R . . . .
H2B H 0.043627 0.659714 0.899294 0.033 Uiso 1 1 calc R . . . .
C3 C -0.3421(4) 0.5271(3) 0.9050(2) 0.0329(8) Uani 1 1 d . . . . .
H3A H -0.405646 0.507640 0.874858 0.039 Uiso 1 1 calc R . . . .
H3B H -0.391144 0.560929 0.942154 0.039 Uiso 1 1 calc R . . . .
C4 C -0.2788(4) 0.4382(3) 0.9474(2) 0.0350(8) Uani 1 1 d . . . . .
H4A H -0.231297 0.454551 0.986543 0.042 Uiso 1 1 calc R . . . .
H4B H -0.346795 0.387661 0.972926 0.042 Uiso 1 1 calc R . . . .
C5 C -0.3016(4) 0.6699(3) 0.8003(2) 0.0319(8) Uani 1 1 d . . . . .
H5A H -0.234443 0.717798 0.770555 0.048 Uiso 1 1 calc GR . . . .
H5B H -0.368697 0.701566 0.830060 0.048 Uiso 1 1 calc GR . . . .
H5C H -0.343354 0.640706 0.765453 0.048 Uiso 1 1 calc GR . . . .
C6 C 0.2155(4) 0.4113(3) 0.6713(2) 0.0323(8) Uani 1 1 d . . . . .
H6A H 0.254280 0.360624 0.645854 0.039 Uiso 1 1 calc R . . . .
H6B H 0.216040 0.472329 0.632019 0.039 Uiso 1 1 calc R . . . .
C7 C 0.3187(5) 0.3310(3) 0.7819(3) 0.0409(10) Uani 1 1 d . . . . .
H7A H 0.402996 0.304009 0.762435 0.049 Uiso 1 1 calc R . . . .
H7B H 0.246304 0.284815 0.783239 0.049 Uiso 1 1 calc R . . . .
C8 C 0.3230(5) 0.3450(3) 0.8614(2) 0.0390(9) Uani 1 1 d . . . . .
H8A H 0.321880 0.281440 0.897801 0.047 Uiso 1 1 calc R . . . .
H8B H 0.405153 0.380445 0.862204 0.047 Uiso 1 1 calc R . . . .
C9 C 0.4222(4) 0.4734(3) 0.6908(2) 0.0340(8) Uani 1 1 d . . . . .
H9A H 0.404211 0.538628 0.662881 0.051 Uiso 1 1 calc GR . . . .
H9B H 0.465082 0.436641 0.654765 0.051 Uiso 1 1 calc GR . . . .
H9C H 0.480514 0.477624 0.728116 0.051 Uiso 1 1 calc GR . . . .
C10 C 0.0577(4) 0.6419(2) 0.6783(2) 0.0248(7) Uani 1 1 d . . . . .
C11 C 0.0740(4) 0.7261(3) 0.6103(2) 0.0299(7) Uani 1 1 d . . . . .
C12 C -0.0338(5) 0.7551(3) 0.5724(3) 0.0429(10) Uani 1 1 d . . . . .
H12 H -0.116933 0.722196 0.588842 0.051 Uiso 1 1 calc R . . . .
C13 C -0.0160(5) 0.8338(4) 0.5098(3) 0.0532(13) Uani 1 1 d . . . . .
C14 C 0.1030(5) 0.8841(3) 0.4842(3) 0.0469(11) Uani 1 1 d . . . . .
H14 H 0.113252 0.936931 0.440885 0.056 Uiso 1 1 calc R . . . .
C15 C 0.2064(4) 0.8544(3) 0.5242(2) 0.0338(8) Uani 1 1 d . . . . .
C16 C 0.1949(4) 0.7750(3) 0.5860(2) 0.0290(7) Uani 1 1 d . . . . .
H16 H 0.268702 0.754453 0.611150 0.035 Uiso 1 1 calc R . . . .
C31 C 0.0752(4) 0.3825(3) 0.7083(2) 0.0298(7) Uani 1 1 d . . . . .
H31A H 0.014533 0.401921 0.670149 0.036 Uiso 1 1 calc R . . . .
H31B H 0.067642 0.311526 0.727358 0.036 Uiso 1 1 calc R . . . .
Cr51 Cr 0.42374(5) -0.00050(4) 0.80753(3) 0.01835(13) Uani 1 1 d . . . . .
Cr52 Cr 0.71478(5) 0.00324(4) 0.80111(3) 0.01977(13) Uani 1 1 d . . . . .
Cl51 Cl 0.24607(8) 0.08683(6) 0.84514(5) 0.02611(17) Uani 1 1 d . . . . .
Cl52 Cl 0.89420(8) -0.04292(7) 0.72546(5) 0.03148(19) Uani 1 1 d . . . . .
Cl53 Cl 0.37442(10) 0.36310(7) 0.47336(6) 0.0382(2) Uani 1 1 d . . . . .
Cl54 Cl 0.86167(10) 0.44096(8) 0.52212(6) 0.0412(2) Uani 1 1 d . . . . .
O51 O 0.5781(2) -0.07301(17) 0.77530(13) 0.0220(5) Uani 1 1 d . . . . .
O52 O 0.3574(2) -0.11088(17) 0.89413(14) 0.0225(5) Uani 1 1 d D . . . .
H52 H 0.411(4) -0.144(3) 0.919(2) 0.027 Uiso 1 1 d DR . . . .
O53 O 0.5563(2) 0.04134(17) 0.86131(13) 0.0225(5) Uani 1 1 d . . . . .
O54 O 0.7504(2) -0.10184(18) 0.88929(14) 0.0258(5) Uani 1 1 d D . . . .
H54 H 0.691(4) -0.144(3) 0.908(3) 0.031 Uiso 1 1 d DR . . . .
O55 O 0.4752(2) 0.10598(17) 0.71635(14) 0.0229(5) Uani 1 1 d . . . . .
O56 O 0.6940(2) 0.11555(17) 0.71647(14) 0.0241(5) Uani 1 1 d . . . . .
N51 N 0.3280(3) -0.0788(2) 0.74583(16) 0.0223(5) Uani 1 1 d . . . . .
N52 N 0.8085(3) 0.0894(2) 0.85830(17) 0.0258(6) Uani 1 1 d . . . . .
C51 C 0.4278(4) -0.1451(3) 0.7169(2) 0.0270(7) Uani 1 1 d . . . . .
H51A H 0.408210 -0.156027 0.667778 0.032 Uiso 1 1 calc R . . . .
H51B H 0.423059 -0.208246 0.754082 0.032 Uiso 1 1 calc R . . . .
C52 C 0.5653(3) -0.1004(2) 0.70574(19) 0.0242(7) Uani 1 1 d . . . . .
H52A H 0.633158 -0.147815 0.695215 0.029 Uiso 1 1 calc R . . . .
H52B H 0.576136 -0.043259 0.662319 0.029 Uiso 1 1 calc R . . . .
C53 C 0.2195(4) -0.1342(3) 0.8029(2) 0.0302(7) Uani 1 1 d . . . . .
H53A H 0.183449 -0.184891 0.781677 0.036 Uiso 1 1 calc R . . . .
H53B H 0.147125 -0.090157 0.813628 0.036 Uiso 1 1 calc R . . . .
C54 C 0.2706(4) -0.1806(3) 0.8765(2) 0.0317(8) Uani 1 1 d . . . . .
H54A H 0.195805 -0.199365 0.918657 0.038 Uiso 1 1 calc R . . . .
H54B H 0.319842 -0.239389 0.870524 0.038 Uiso 1 1 calc R . . . .
C55 C 0.2690(4) -0.0173(3) 0.6817(2) 0.0281(7) Uani 1 1 d . . . . .
H55A H 0.214756 0.031992 0.700532 0.042 Uiso 1 1 calc GR . . . .
H55B H 0.213676 -0.057697 0.661050 0.042 Uiso 1 1 calc GR . . . .
H55C H 0.339654 0.014076 0.641376 0.042 Uiso 1 1 calc GR . . . .
C56 C 0.7034(4) 0.1326(3) 0.9074(2) 0.0316(8) Uani 1 1 d . . . . .
H56A H 0.730597 0.199141 0.907594 0.038 Uiso 1 1 calc R . . . .
H56B H 0.692284 0.093749 0.960652 0.038 Uiso 1 1 calc R . . . .
C57 C 0.5734(4) 0.1346(3) 0.8764(2) 0.0291(7) Uani 1 1 d . . . . .
H57A H 0.499563 0.147560 0.914322 0.035 Uiso 1 1 calc R . . . .
H57B H 0.576415 0.185594 0.828827 0.035 Uiso 1 1 calc R . . . .
C58 C 0.8886(4) 0.0203(3) 0.9086(2) 0.0334(8) Uani 1 1 d . . . . .
H58A H 0.968851 0.002862 0.877349 0.040 Uiso 1 1 calc R . . . .
H58B H 0.916560 0.051630 0.947303 0.040 Uiso 1 1 calc R . . . .
C59 C 0.8070(4) -0.0693(3) 0.9479(2) 0.0360(8) Uani 1 1 d . . . . .
H59A H 0.863100 -0.119827 0.973453 0.043 Uiso 1 1 calc R . . . .
H59B H 0.736215 -0.054663 0.986904 0.043 Uiso 1 1 calc R . . . .
C60 C 0.8968(4) 0.1661(3) 0.8067(2) 0.0340(8) Uani 1 1 d . . . . .
H60A H 0.954776 0.138346 0.769551 0.051 Uiso 1 1 calc GR . . . .
H60B H 0.950537 0.194510 0.836793 0.051 Uiso 1 1 calc GR . . . .
H60C H 0.843528 0.216361 0.779657 0.051 Uiso 1 1 calc GR . . . .
C61 C 0.5876(3) 0.1442(2) 0.69200(19) 0.0223(6) Uani 1 1 d . . . . .
C62 C 0.5974(4) 0.2317(2) 0.62729(19) 0.0239(6) Uani 1 1 d . . . . .
C63 C 0.4913(3) 0.2548(2) 0.5868(2) 0.0243(6) Uani 1 1 d . . . . .
H63 H 0.412556 0.216070 0.600456 0.029 Uiso 1 1 calc R . . . .
C64 C 0.5029(4) 0.3353(3) 0.5263(2) 0.0279(7) Uani 1 1 d . . . . .
C65 C 0.6156(4) 0.3936(3) 0.5066(2) 0.0299(7) Uani 1 1 d . . . . .
H65 H 0.622037 0.448885 0.465363 0.036 Uiso 1 1 calc R . . . .
C66 C 0.7189(4) 0.3699(3) 0.5480(2) 0.0289(7) Uani 1 1 d . . . . .
C67 C 0.7132(3) 0.2891(3) 0.6080(2) 0.0258(7) Uani 1 1 d . . . . .
H67 H 0.785664 0.273062 0.635219 0.031 Uiso 1 1 calc R . . . .
Cl5 Cl -0.00671(9) 0.26430(6) 0.96521(5) 0.03141(19) Uani 1 1 d . . . . .
Cl55 Cl 0.54096(9) -0.24501(6) 0.97021(5) 0.02795(18) 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 2.2960(10) . ?
Cr1 O1 1.964(3) . ?
Cr1 O2 1.997(3) . ?
Cr1 O3 1.959(2) . ?
Cr1 O5 1.988(3) . ?
Cr1 N1 2.098(3) . ?
Cr2 Cl2 2.2930(10) . ?
Cr2 O1 1.944(2) . ?
Cr2 O3 1.954(2) . ?
Cr2 O4 2.004(2) . ?
Cr2 O6 1.988(2) . ?
Cr2 N2 2.093(3) . ?
Cl3 C13 1.730(5) . ?
Cl4 C15 1.738(4) . ?
O1 C2 1.436(4) . ?
O2 H2 0.824(19) . ?
O2 C4 1.456(4) . ?
O3 C31 1.424(4) . ?
O4 H4 0.833(19) . ?
O4 C8 1.446(5) . ?
O5 C10 1.256(5) . ?
O6 C10 1.271(4) . ?
N1 C1 1.510(5) . ?
N1 C3 1.496(5) . ?
N1 C5 1.487(5) . ?
N2 C6 1.508(5) . ?
N2 C7 1.472(5) . ?
N2 C9 1.473(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.511(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.516(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C31 1.512(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.510(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.502(5) . ?
C11 C12 1.397(6) . ?
C11 C16 1.389(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.394(6) . ?
C13 C14 1.383(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.381(7) . ?
C15 C16 1.391(5) . ?
C16 H16 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
Cr51 Cl51 2.2973(9) . ?
Cr51 O51 1.965(2) . ?
Cr51 O52 1.996(2) . ?
Cr51 O53 1.958(2) . ?
Cr51 O55 1.983(2) . ?
Cr51 N51 2.094(3) . ?
Cr52 Cl52 2.3067(9) . ?
Cr52 O51 1.954(2) . ?
Cr52 O53 1.960(2) . ?
Cr52 O54 2.001(2) . ?
Cr52 O56 1.983(2) . ?
Cr52 N52 2.100(3) . ?
Cl53 C64 1.734(4) . ?
Cl54 C66 1.730(4) . ?
O51 C52 1.429(4) . ?
O52 H52 0.835(19) . ?
O52 C54 1.458(4) . ?
O53 C57 1.432(4) . ?
O54 H54 0.835(19) . ?
O54 C59 1.450(5) . ?
O55 C61 1.252(4) . ?
O56 C61 1.265(4) . ?
N51 C51 1.499(4) . ?
N51 C53 1.496(4) . ?
N51 C55 1.491(4) . ?
N52 C56 1.510(5) . ?
N52 C58 1.506(5) . ?
N52 C60 1.480(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.518(5) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.516(5) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.519(5) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.504(6) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.498(5) . ?
C62 C63 1.396(5) . ?
C62 C67 1.401(5) . ?
C63 H63 0.9500 . ?
C63 C64 1.388(5) . ?
C64 C65 1.383(5) . ?
C65 H65 0.9500 . ?
C65 C66 1.383(6) . ?
C66 C67 1.387(5) . ?
C67 H67 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
O1 Cr1 Cl1 176.66(8) . . ?
O1 Cr1 O2 92.04(11) . . ?
O1 Cr1 O5 89.79(11) . . ?
O1 Cr1 N1 82.76(11) . . ?
O2 Cr1 Cl1 89.14(8) . . ?
O2 Cr1 N1 81.94(11) . . ?
O3 Cr1 Cl1 98.19(8) . . ?
O3 Cr1 O1 78.61(10) . . ?
O3 Cr1 O2 94.19(10) . . ?
O3 Cr1 O5 91.54(10) . . ?
O3 Cr1 N1 160.83(11) . . ?
O5 Cr1 Cl1 89.34(8) . . ?
O5 Cr1 O2 174.22(11) . . ?
O5 Cr1 N1 92.86(11) . . ?
N1 Cr1 Cl1 100.50(9) . . ?
O1 Cr2 Cl2 100.24(8) . . ?
O1 Cr2 O3 79.20(10) . . ?
O1 Cr2 O4 94.40(11) . . ?
O1 Cr2 O6 91.95(10) . . ?
O1 Cr2 N2 160.09(11) . . ?
O3 Cr2 Cl2 179.42(8) . . ?
O3 Cr2 O4 92.05(11) . . ?
O3 Cr2 O6 90.72(11) . . ?
O3 Cr2 N2 81.11(11) . . ?
O4 Cr2 Cl2 87.81(8) . . ?
O4 Cr2 N2 83.37(11) . . ?
O6 Cr2 Cl2 89.48(8) . . ?
O6 Cr2 O4 173.44(11) . . ?
O6 Cr2 N2 91.20(11) . . ?
N2 Cr2 Cl2 99.43(9) . . ?
Cr2 O1 Cr1 98.38(11) . . ?
C2 O1 Cr1 111.1(2) . . ?
C2 O1 Cr2 129.6(2) . . ?
Cr1 O2 H2 119(3) . . ?
C4 O2 Cr1 116.1(2) . . ?
C4 O2 H2 107(4) . . ?
Cr2 O3 Cr1 98.24(11) . . ?
C31 O3 Cr1 132.4(2) . . ?
C31 O3 Cr2 117.3(2) . . ?
Cr2 O4 H4 113(3) . . ?
C8 O4 Cr2 110.5(2) . . ?
C8 O4 H4 111(3) . . ?
C10 O5 Cr1 127.9(2) . . ?
C10 O6 Cr2 126.6(2) . . ?
C1 N1 Cr1 107.5(2) . . ?
C3 N1 Cr1 105.3(2) . . ?
C3 N1 C1 110.1(3) . . ?
C5 N1 Cr1 114.0(2) . . ?
C5 N1 C1 110.2(3) . . ?
C5 N1 C3 109.7(3) . . ?
C6 N2 Cr2 103.4(2) . . ?
C7 N2 Cr2 107.8(2) . . ?
C7 N2 C6 110.9(3) . . ?
C7 N2 C9 112.1(3) . . ?
C9 N2 Cr2 114.6(2) . . ?
C9 N2 C6 107.7(3) . . ?
N1 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
N1 C1 C2 110.0(3) . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
O1 C2 C1 106.3(3) . . ?
O1 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N1 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
N1 C3 C4 110.0(3) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
O2 C4 C3 106.4(3) . . ?
O2 C4 H4A 110.5 . . ?
O2 C4 H4B 110.5 . . ?
C3 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
H4A C4 H4B 108.6 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
N2 C6 C31 109.9(3) . . ?
H6A C6 H6B 108.2 . . ?
C31 C6 H6A 109.7 . . ?
C31 C6 H6B 109.7 . . ?
N2 C7 H7A 109.8 . . ?
N2 C7 H7B 109.8 . . ?
N2 C7 C8 109.5(3) . . ?
H7A C7 H7B 108.2 . . ?
C8 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
O4 C8 C7 108.8(3) . . ?
O4 C8 H8A 109.9 . . ?
O4 C8 H8B 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5 C10 O6 125.9(3) . . ?
O5 C10 C11 117.7(3) . . ?
O6 C10 C11 116.4(3) . . ?
C12 C11 C10 119.4(4) . . ?
C16 C11 C10 120.2(3) . . ?
C16 C11 C12 120.5(4) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 C11 118.1(4) . . ?
C13 C12 H12 120.9 . . ?
C12 C13 Cl3 118.5(4) . . ?
C14 C13 Cl3 118.6(4) . . ?
C14 C13 C12 122.9(4) . . ?
C13 C14 H14 121.4 . . ?
C15 C14 C13 117.2(4) . . ?
C15 C14 H14 121.4 . . ?
C14 C15 Cl4 118.8(3) . . ?
C14 C15 C16 122.3(4) . . ?
C16 C15 Cl4 118.9(3) . . ?
C11 C16 C15 119.0(4) . . ?
C11 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
O3 C31 C6 109.7(3) . . ?
O3 C31 H31A 109.7 . . ?
O3 C31 H31B 109.7 . . ?
C6 C31 H31A 109.7 . . ?
C6 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
O51 Cr51 Cl51 178.85(8) . . ?
O51 Cr51 O52 91.84(10) . . ?
O51 Cr51 O55 89.80(10) . . ?
O51 Cr51 N51 83.30(11) . . ?
O52 Cr51 Cl51 88.89(7) . . ?
O52 Cr51 N51 82.28(11) . . ?
O53 Cr51 Cl51 100.41(7) . . ?
O53 Cr51 O51 78.65(10) . . ?
O53 Cr51 O52 93.86(10) . . ?
O53 Cr51 O55 91.79(10) . . ?
O53 Cr51 N51 161.43(11) . . ?
O55 Cr51 Cl51 89.56(7) . . ?
O55 Cr51 O52 174.32(10) . . ?
O55 Cr51 N51 92.51(11) . . ?
N51 Cr51 Cl51 97.68(8) . . ?
O51 Cr52 Cl52 98.40(7) . . ?
O51 Cr52 O53 78.87(10) . . ?
O51 Cr52 O54 93.20(10) . . ?
O51 Cr52 O56 92.80(10) . . ?
O51 Cr52 N52 160.38(11) . . ?
O53 Cr52 Cl52 176.86(8) . . ?
O53 Cr52 O54 91.76(10) . . ?
O53 Cr52 O56 89.38(10) . . ?
O53 Cr52 N52 82.14(11) . . ?
O54 Cr52 Cl52 89.94(8) . . ?
O54 Cr52 N52 82.42(12) . . ?
O56 Cr52 Cl52 89.21(8) . . ?
O56 Cr52 O54 174.00(11) . . ?
O56 Cr52 N52 91.90(11) . . ?
N52 Cr52 Cl52 100.71(9) . . ?
Cr52 O51 Cr51 98.32(10) . . ?
C52 O51 Cr51 110.7(2) . . ?
C52 O51 Cr52 131.1(2) . . ?
Cr51 O52 H52 120(3) . . ?
C54 O52 Cr51 115.7(2) . . ?
C54 O52 H52 105(3) . . ?
Cr51 O53 Cr52 98.40(11) . . ?
C57 O53 Cr51 128.1(2) . . ?
C57 O53 Cr52 111.6(2) . . ?
Cr52 O54 H54 117(3) . . ?
C59 O54 Cr52 114.9(2) . . ?
C59 O54 H54 112(3) . . ?
C61 O55 Cr51 127.4(2) . . ?
C61 O56 Cr52 126.8(2) . . ?
C51 N51 Cr51 106.9(2) . . ?
C53 N51 Cr51 104.8(2) . . ?
C53 N51 C51 111.4(3) . . ?
C55 N51 Cr51 114.0(2) . . ?
C55 N51 C51 110.9(3) . . ?
C55 N51 C53 108.7(3) . . ?
C56 N52 Cr52 108.3(2) . . ?
C58 N52 Cr52 105.0(2) . . ?
C58 N52 C56 109.5(3) . . ?
C60 N52 Cr52 113.9(2) . . ?
C60 N52 C56 110.5(3) . . ?
C60 N52 C58 109.5(3) . . ?
N51 C51 H51A 109.7 . . ?
N51 C51 H51B 109.7 . . ?
N51 C51 C52 109.6(3) . . ?
H51A C51 H51B 108.2 . . ?
C52 C51 H51A 109.7 . . ?
C52 C51 H51B 109.7 . . ?
O51 C52 C51 106.3(3) . . ?
O51 C52 H52A 110.5 . . ?
O51 C52 H52B 110.5 . . ?
C51 C52 H52A 110.5 . . ?
C51 C52 H52B 110.5 . . ?
H52A C52 H52B 108.7 . . ?
N51 C53 H53A 109.6 . . ?
N51 C53 H53B 109.6 . . ?
N51 C53 C54 110.4(3) . . ?
H53A C53 H53B 108.1 . . ?
C54 C53 H53A 109.6 . . ?
C54 C53 H53B 109.6 . . ?
O52 C54 C53 108.4(3) . . ?
O52 C54 H54A 110.0 . . ?
O52 C54 H54B 110.0 . . ?
C53 C54 H54A 110.0 . . ?
C53 C54 H54B 110.0 . . ?
H54A C54 H54B 108.4 . . ?
N51 C55 H55A 109.5 . . ?
N51 C55 H55B 109.5 . . ?
N51 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N52 C56 H56A 109.7 . . ?
N52 C56 H56B 109.7 . . ?
N52 C56 C57 109.8(3) . . ?
H56A C56 H56B 108.2 . . ?
C57 C56 H56A 109.7 . . ?
C57 C56 H56B 109.7 . . ?
O53 C57 C56 106.3(3) . . ?
O53 C57 H57A 110.5 . . ?
O53 C57 H57B 110.5 . . ?
C56 C57 H57A 110.5 . . ?
C56 C57 H57B 110.5 . . ?
H57A C57 H57B 108.7 . . ?
N52 C58 H58A 109.7 . . ?
N52 C58 H58B 109.7 . . ?
H58A C58 H58B 108.2 . . ?
C59 C58 N52 109.7(3) . . ?
C59 C58 H58A 109.7 . . ?
C59 C58 H58B 109.7 . . ?
O54 C59 C58 106.9(3) . . ?
O54 C59 H59A 110.3 . . ?
O54 C59 H59B 110.3 . . ?
C58 C59 H59A 110.3 . . ?
C58 C59 H59B 110.3 . . ?
H59A C59 H59B 108.6 . . ?
N52 C60 H60A 109.5 . . ?
N52 C60 H60B 109.5 . . ?
N52 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O55 C61 O56 126.3(3) . . ?
O55 C61 C62 116.9(3) . . ?
O56 C61 C62 116.8(3) . . ?
C63 C62 C61 119.6(3) . . ?
C63 C62 C67 120.9(3) . . ?
C67 C62 C61 119.5(3) . . ?
C62 C63 H63 120.6 . . ?
C64 C63 C62 118.8(3) . . ?
C64 C63 H63 120.6 . . ?
C63 C64 Cl53 119.5(3) . . ?
C65 C64 Cl53 119.0(3) . . ?
C65 C64 C63 121.4(3) . . ?
C64 C65 H65 120.6 . . ?
C64 C65 C66 118.8(3) . . ?
C66 C65 H65 120.6 . . ?
C65 C66 Cl54 118.9(3) . . ?
C65 C66 C67 122.0(3) . . ?
C67 C66 Cl54 119.0(3) . . ?
C62 C67 H67 120.9 . . ?
C66 C67 C62 118.1(3) . . ?
C66 C67 H67 120.9 . . ?

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 H2 Cl5 0.824(19) 2.12(2) 2.942(3) 174(5) .
O4 H4 Cl5 0.833(19) 2.11(2) 2.932(3) 170(5) .
O52 H52 Cl55 0.835(19) 2.10(2) 2.927(3) 169(5) .
O54 H54 Cl55 0.835(19) 2.12(2) 2.950(3) 172(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 C2 C1 49.3(3) . . . . ?
Cr1 O2 C4 C3 26.7(4) . . . . ?
Cr1 O3 C31 C6 129.6(3) . . . . ?
Cr1 O5 C10 O6 0.7(5) . . . . ?
Cr1 O5 C10 C11 -178.4(2) . . . . ?
Cr1 N1 C1 C2 25.5(3) . . . . ?
Cr1 N1 C3 C4 45.4(4) . . . . ?
Cr2 O1 C2 C1 170.8(2) . . . . ?
Cr2 O3 C31 C6 -4.0(4) . . . . ?
Cr2 O4 C8 C7 -40.8(4) . . . . ?
Cr2 O6 C10 O5 -4.4(5) . . . . ?
Cr2 O6 C10 C11 174.7(2) . . . . ?
Cr2 N2 C6 C31 -45.5(3) . . . . ?
Cr2 N2 C7 C8 -33.8(4) . . . . ?
Cl3 C13 C14 C15 178.9(4) . . . . ?
Cl4 C15 C16 C11 177.1(3) . . . . ?
O5 C10 C11 C12 -12.3(6) . . . . ?
O5 C10 C11 C16 167.2(3) . . . . ?
O6 C10 C11 C12 168.5(4) . . . . ?
O6 C10 C11 C16 -12.0(5) . . . . ?
N1 C1 C2 O1 -48.3(4) . . . . ?
N1 C3 C4 O2 -47.5(4) . . . . ?
N2 C6 C31 O3 34.1(4) . . . . ?
N2 C7 C8 O4 49.8(5) . . . . ?
C1 N1 C3 C4 -70.2(4) . . . . ?
C3 N1 C1 C2 139.7(3) . . . . ?
C5 N1 C1 C2 -99.2(3) . . . . ?
C5 N1 C3 C4 168.4(3) . . . . ?
C6 N2 C7 C8 -146.4(4) . . . . ?
C7 N2 C6 C31 69.9(4) . . . . ?
C9 N2 C6 C31 -167.2(3) . . . . ?
C9 N2 C7 C8 93.2(4) . . . . ?
C10 C11 C12 C13 179.7(5) . . . . ?
C10 C11 C16 C15 -178.2(3) . . . . ?
C11 C12 C13 Cl3 179.8(4) . . . . ?
C11 C12 C13 C14 -0.3(9) . . . . ?
C12 C11 C16 C15 1.2(6) . . . . ?
C12 C13 C14 C15 -1.0(9) . . . . ?
C13 C14 C15 Cl4 -177.3(4) . . . . ?
C13 C14 C15 C16 2.5(7) . . . . ?
C14 C15 C16 C11 -2.7(6) . . . . ?
C16 C11 C12 C13 0.2(7) . . . . ?
Cr51 O51 C52 C51 -48.6(3) . . . . ?
Cr51 O52 C54 C53 -17.5(4) . . . . ?
Cr51 O53 C57 C56 -170.6(2) . . . . ?
Cr51 O55 C61 O56 7.8(5) . . . . ?
Cr51 O55 C61 C62 -172.7(2) . . . . ?
Cr51 N51 C51 C52 -28.6(3) . . . . ?
Cr51 N51 C53 C54 -45.5(3) . . . . ?
Cr52 O51 C52 C51 -170.8(2) . . . . ?
Cr52 O53 C57 C56 -49.8(3) . . . . ?
Cr52 O54 C59 C58 -30.5(4) . . . . ?
Cr52 O56 C61 O55 -0.8(5) . . . . ?
Cr52 O56 C61 C62 179.7(2) . . . . ?
Cr52 N52 C56 C57 -22.8(4) . . . . ?
Cr52 N52 C58 C59 -44.4(4) . . . . ?
Cl53 C64 C65 C66 -178.6(3) . . . . ?
Cl54 C66 C67 C62 -179.1(3) . . . . ?
O55 C61 C62 C63 -13.4(5) . . . . ?
O55 C61 C62 C67 166.9(3) . . . . ?
O56 C61 C62 C63 166.2(3) . . . . ?
O56 C61 C62 C67 -13.6(5) . . . . ?
N51 C51 C52 O51 50.5(3) . . . . ?
N51 C53 C54 O52 42.2(4) . . . . ?
N52 C56 C57 O53 46.4(4) . . . . ?
N52 C58 C59 O54 49.6(4) . . . . ?
C51 N51 C53 C54 69.8(4) . . . . ?
C53 N51 C51 C52 -142.6(3) . . . . ?
C55 N51 C51 C52 96.2(3) . . . . ?
C55 N51 C53 C54 -167.7(3) . . . . ?
C56 N52 C58 C59 71.7(4) . . . . ?
C58 N52 C56 C57 -136.8(3) . . . . ?
C60 N52 C56 C57 102.5(4) . . . . ?
C60 N52 C58 C59 -167.0(3) . . . . ?
C61 C62 C63 C64 -179.0(3) . . . . ?
C61 C62 C67 C66 -179.7(3) . . . . ?
C62 C63 C64 Cl53 178.0(3) . . . . ?
C62 C63 C64 C65 -1.3(6) . . . . ?
C63 C62 C67 C66 0.6(5) . . . . ?
C63 C64 C65 C66 0.7(6) . . . . ?
C64 C65 C66 Cl54 178.5(3) . . . . ?
C64 C65 C66 C67 0.7(6) . . . . ?
C65 C66 C67 C62 -1.3(6) . . . . ?
C67 C62 C63 C64 0.7(5) . . . . ?

_olex2_date_sample_data_collection 2017-06-07
_olex2_date_sample_submission    2017-05-29
_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 900o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.906
_oxdiff_exptl_absorpt_empirical_full_min 0.642
####################################################################### 
# 
# 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 1579645'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
# local name eb16270

_audit_creation_date             2016-11-25
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H29 Cl2 Cr2 N2 O6, Cl'
_chemical_formula_sum            'C17 H29 Cl3 Cr2 N2 O6'
_chemical_formula_weight         567.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl Na'
_chemical_oxdiff_usercomment     '@ 120 K L145'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.1908(3)
_cell_length_b                   10.41623(19)
_cell_length_c                   14.1087(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.560(2)
_cell_angle_gamma                90
_cell_volume                     2331.11(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22700
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.0080
_cell_measurement_theta_min      3.9730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
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            'dark purple'
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
22 -3 1 0.0911
-3 7 17 0.2302
-22 3 0 0.0932
2 13 -10 0.1278
-2 -13 10 0.1278
-6 8 16 0.2234
-4 -7 -16 0.2069
-1 -11 -12 0.2084
-12 -13 2 0.1648
-15 -9 10 0.1393
15 10 -9 0.1496
13 -1 -18 0.2250
-2 -2 -19 0.2137
14 -9 8 0.1116
-12 11 10 0.2073

_exptl_crystal_recrystallization_method 
'The material was recrystallised from acetonitrile by hydrothermal bomb'
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.194
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
21.9563 -3.0054 1.0230 0.9556 0.3065 0.1522
-3.0143 6.9895 16.9787 0.1252 0.0460 -0.9685
-21.9578 3.0053 -0.0242 -0.9443 -0.2792 -0.1941
2.0232 12.9797 -9.9804 0.0985 -1.0113 -0.0265
-2.0232 -12.9797 9.9804 -0.0985 1.0113 0.0265
-6.0065 7.9894 15.9769 -0.0093 -0.0533 -0.9737
-3.9746 -6.9864 -15.9880 -0.4234 -0.0527 0.8982
-0.9897 -10.9819 -11.9910 -0.2834 0.3012 0.8824
-11.9931 -12.9747 1.9786 -0.6308 0.7448 0.3210
-14.9963 -8.9800 9.9670 -0.6354 0.7181 -0.1659
14.9957 9.9784 -8.9678 0.6561 -0.7484 0.0891
13.0032 -1.0032 -17.9636 0.3623 -0.3703 0.8417
-1.9692 -1.9948 -18.9801 -0.3216 -0.4126 0.8576
13.9547 -8.9930 8.0029 0.6242 0.8040 0.0358
-11.9840 10.9879 9.9784 -0.3139 -0.4187 -0.8514

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48698
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.306
_diffrn_reflns_theta_min         2.970
_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 0.937
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  27.00   1.00    4.00    --  -13.24 -99.00 -60.00   47
  2  ω    -20.00  27.00   1.00    4.00    --  -13.24 -99.00 120.00   47
  3  ω     -8.00  87.00   1.00    4.00    --   14.65  38.00 -90.00   95
  4  ω     35.00 101.00   1.00    4.00    --   14.65 178.00-150.00   66
  5  ω    -58.00  37.00   1.00    4.00    --   14.65 -38.00 150.00   95
  6  ω     35.00 101.00   1.00    4.00    --   14.65 178.00 150.00   66
  7  ω    -20.00  55.00   1.00    4.00    --   14.65 -99.00 150.00   75
  8  ω     -8.00  87.00   1.00    4.00    --   14.65  38.00   0.00   95
  9  ω    -40.00  57.00   1.00    4.00    --  -13.24  57.00 -60.00   97
 10  ω     -8.00  19.00   1.00    4.00    --   14.65  38.00 120.00   27
;
_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      0.0442823000
_diffrn_orient_matrix_UB_12      0.0094161000
_diffrn_orient_matrix_UB_13      0.0113576000
_diffrn_orient_matrix_UB_21      0.0047942000
_diffrn_orient_matrix_UB_22      -0.0576691000
_diffrn_orient_matrix_UB_23      0.0273035000
_diffrn_orient_matrix_UB_31      0.0041044000
_diffrn_orient_matrix_UB_32      -0.0349292000
_diffrn_orient_matrix_UB_33      -0.0419367000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6488
_reflns_number_total             7156
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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         0.516
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         7156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0286
_refine_ls_restrained_S_all      1.040
_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)+(0.0281P)²+1.5432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0696
_refine_special_details          
;
O-bound H atoms were identified from a difference Fourier map and freely refined.

#===============================================================================
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 ......      2.067 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           7 Note
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          3 Report

Not significant

#===============================================================================
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  Cl1     ..        5.5 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr2    --  Cl2     ..        5.6 s.u.
793_ALERT_4_G The Model has Chirality at N1      (Centro SPGR)          S Verify
793_ALERT_4_G The Model has Chirality at N2      (Centro SPGR)          S Verify
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        471 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
978_ALERT_2_G Number C-C Bonds with Positive Residual Density           8 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:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)
;
_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 0.22151(2) 0.38402(2) 0.47252(2) 0.01130(5) Uani 1 1 d . . . . .
Cr2 Cr 0.21811(2) 0.66664(2) 0.49252(2) 0.00990(5) Uani 1 1 d . . . . .
Cl1 Cl 0.18809(3) 0.20595(3) 0.55327(3) 0.02305(8) Uani 1 1 d . . . . .
Cl2 Cl 0.29402(2) 0.83652(3) 0.45175(3) 0.01848(7) Uani 1 1 d . . . . .
O1 O 0.25140(6) 0.53745(9) 0.40581(7) 0.01189(18) Uani 1 1 d . . . . .
O2 O 0.12579(7) 0.34263(10) 0.36392(7) 0.0155(2) Uani 1 1 d . . . . .
H2 H 0.0970(13) 0.396(2) 0.3411(16) 0.030(6) Uiso 1 1 d . . . . .
O3 O 0.15686(6) 0.51606(9) 0.52457(7) 0.01272(18) Uani 1 1 d . . . . .
O4 O 0.11888(6) 0.72621(10) 0.39351(7) 0.01469(19) Uani 1 1 d . . . . .
H4 H 0.0964(14) 0.677(2) 0.3564(17) 0.039(6) Uiso 1 1 d . . . . .
O5 O 0.32230(6) 0.40995(10) 0.57609(7) 0.01573(19) Uani 1 1 d . . . . .
O6 O 0.31228(6) 0.62213(9) 0.60116(7) 0.01392(19) Uani 1 1 d . . . . .
N1 N 0.29122(8) 0.29098(11) 0.38223(8) 0.0149(2) Uani 1 1 d . . . . .
N2 N 0.15240(7) 0.76067(11) 0.58558(8) 0.0126(2) Uani 1 1 d . . . . .
C1 C 0.32145(9) 0.39217(14) 0.32129(10) 0.0172(3) Uani 1 1 d . . . . .
H1A H 0.281126 0.400545 0.258820 0.021 Uiso 1 1 calc R . . . .
H1B H 0.376943 0.367239 0.307726 0.021 Uiso 1 1 calc R . . . .
C2 C 0.32906(9) 0.51956(14) 0.37483(10) 0.0154(3) Uani 1 1 d . . . . .
H2A H 0.376659 0.517264 0.431127 0.018 Uiso 1 1 calc R . . . .
H2B H 0.338676 0.590335 0.331470 0.018 Uiso 1 1 calc R . . . .
C3 C 0.22984(10) 0.20282(15) 0.32108(11) 0.0204(3) Uani 1 1 d . . . . .
H3A H 0.219259 0.127579 0.359841 0.025 Uiso 1 1 calc R . . . .
H3B H 0.253705 0.171586 0.265969 0.025 Uiso 1 1 calc R . . . .
C4 C 0.14810(10) 0.27234(16) 0.28370(11) 0.0227(3) Uani 1 1 d . . . . .
H4A H 0.154827 0.332389 0.231386 0.027 Uiso 1 1 calc R . . . .
H4B H 0.103157 0.210060 0.257344 0.027 Uiso 1 1 calc R . . . .
C5 C 0.36324(11) 0.21536(16) 0.43551(12) 0.0255(3) Uani 1 1 d . . . . .
H5A H 0.406017 0.273695 0.470971 0.038 Uiso 1 1 calc GR . . . .
H5B H 0.387776 0.164628 0.389563 0.038 Uiso 1 1 calc GR . . . .
H5C H 0.343574 0.157719 0.481233 0.038 Uiso 1 1 calc GR . . . .
C6 C 0.09822(10) 0.66177(14) 0.62164(11) 0.0183(3) Uani 1 1 d . . . . .
H6A H 0.040819 0.663137 0.580902 0.022 Uiso 1 1 calc R . . . .
H6B H 0.093658 0.682285 0.688914 0.022 Uiso 1 1 calc R . . . .
C7 C 0.13638(10) 0.52981(13) 0.61819(10) 0.0173(3) Uani 1 1 d . . . . .
H7A H 0.187759 0.521279 0.669342 0.021 Uiso 1 1 calc R . . . .
H7B H 0.095626 0.462856 0.628346 0.021 Uiso 1 1 calc R . . . .
C8 C 0.09920(10) 0.85930(14) 0.52441(11) 0.0181(3) Uani 1 1 d . . . . .
H8A H 0.135043 0.931774 0.511759 0.022 Uiso 1 1 calc R . . . .
H8B H 0.056438 0.893072 0.559195 0.022 Uiso 1 1 calc R . . . .
C9 C 0.05595(10) 0.80024(16) 0.42985(11) 0.0214(3) Uani 1 1 d . . . . .
H9A H 0.009251 0.743882 0.439996 0.026 Uiso 1 1 calc R . . . .
H9B H 0.032489 0.868144 0.383049 0.026 Uiso 1 1 calc R . . . .
C10 C 0.20780(10) 0.82605(15) 0.66809(11) 0.0200(3) Uani 1 1 d . . . . .
H10A H 0.238612 0.761620 0.712086 0.030 Uiso 1 1 calc GR . . . .
H10B H 0.173349 0.878520 0.702875 0.030 Uiso 1 1 calc GR . . . .
H10C H 0.248004 0.881153 0.643772 0.030 Uiso 1 1 calc GR . . . .
C11 C 0.34421(9) 0.51233(13) 0.62260(10) 0.0135(2) Uani 1 1 d . . . . .
C12 C 0.41269(8) 0.50235(14) 0.71055(10) 0.0137(2) Uani 1 1 d . . . . .
C13 C 0.47048(9) 0.40128(15) 0.72064(11) 0.0185(3) Uani 1 1 d . . . . .
H13 H 0.466400 0.338080 0.671371 0.022 Uiso 1 1 calc R . . . .
C14 C 0.53384(9) 0.39335(15) 0.80268(11) 0.0201(3) Uani 1 1 d . . . . .
H14 H 0.574032 0.325869 0.808828 0.024 Uiso 1 1 calc R . . . .
C15 C 0.53867(9) 0.48404(14) 0.87605(11) 0.0183(3) Uani 1 1 d . . . . .
H15 H 0.582562 0.479140 0.931808 0.022 Uiso 1 1 calc R . . . .
C16 C 0.47927(9) 0.58165(14) 0.86764(10) 0.0176(3) Uani 1 1 d . . . . .
H16 H 0.481255 0.641647 0.918765 0.021 Uiso 1 1 calc R . . . .
C17 C 0.41694(9) 0.59169(13) 0.78459(10) 0.0149(3) Uani 1 1 d . . . . .
H17 H 0.377141 0.659730 0.778354 0.018 Uiso 1 1 calc R . . . .
Cl3 Cl 0.02289(2) 0.54547(3) 0.25340(2) 0.01776(7) 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 2.2975(4) . ?
Cr1 O1 1.9638(10) . ?
Cr1 O2 1.9959(11) . ?
Cr1 O3 1.9583(10) . ?
Cr1 O5 1.9788(10) . ?
Cr1 N1 2.1005(12) . ?
Cr2 Cl2 2.2926(4) . ?
Cr2 O1 1.9653(9) . ?
Cr2 O3 1.9564(10) . ?
Cr2 O4 2.0044(10) . ?
Cr2 O6 1.9881(10) . ?
Cr2 N2 2.0915(11) . ?
O1 C2 1.4238(16) . ?
O2 H2 0.76(2) . ?
O2 C4 1.4529(17) . ?
O3 C7 1.4320(16) . ?
O4 H4 0.77(2) . ?
O4 C9 1.4509(18) . ?
O5 C11 1.2650(17) . ?
O6 C11 1.2665(16) . ?
N1 C1 1.5028(18) . ?
N1 C3 1.4939(19) . ?
N1 C5 1.4811(19) . ?
N2 C6 1.5062(18) . ?
N2 C8 1.4981(18) . ?
N2 C10 1.4849(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.520(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.508(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.512(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.508(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.4928(19) . ?
C12 C13 1.3967(19) . ?
C12 C17 1.3904(19) . ?
C13 H13 0.9500 . ?
C13 C14 1.387(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.392(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.389(2) . ?
C17 H17 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
O1 Cr1 Cl1 178.90(3) . . ?
O1 Cr1 O2 92.06(4) . . ?
O1 Cr1 O5 89.82(4) . . ?
O1 Cr1 N1 82.58(4) . . ?
O2 Cr1 Cl1 89.00(3) . . ?
O2 Cr1 N1 82.17(4) . . ?
O3 Cr1 Cl1 100.62(3) . . ?
O3 Cr1 O1 79.03(4) . . ?
O3 Cr1 O2 92.78(4) . . ?
O3 Cr1 O5 92.91(4) . . ?
O3 Cr1 N1 160.75(4) . . ?
O5 Cr1 Cl1 89.16(3) . . ?
O5 Cr1 O2 174.25(4) . . ?
O5 Cr1 N1 92.70(4) . . ?
N1 Cr1 Cl1 97.86(4) . . ?
O1 Cr2 Cl2 98.31(3) . . ?
O1 Cr2 O4 93.42(4) . . ?
O1 Cr2 O6 93.24(4) . . ?
O1 Cr2 N2 161.60(4) . . ?
O3 Cr2 Cl2 177.21(3) . . ?
O3 Cr2 O1 79.04(4) . . ?
O3 Cr2 O4 92.10(4) . . ?
O3 Cr2 O6 88.90(4) . . ?
O3 Cr2 N2 83.41(4) . . ?
O4 Cr2 Cl2 88.93(3) . . ?
O4 Cr2 N2 81.67(4) . . ?
O6 Cr2 Cl2 90.38(3) . . ?
O6 Cr2 O4 173.33(4) . . ?
O6 Cr2 N2 91.91(4) . . ?
N2 Cr2 Cl2 99.31(3) . . ?
Cr1 O1 Cr2 97.72(4) . . ?
C2 O1 Cr1 110.99(8) . . ?
C2 O1 Cr2 130.54(8) . . ?
Cr1 O2 H2 119.1(17) . . ?
C4 O2 Cr1 115.52(9) . . ?
C4 O2 H2 105.5(17) . . ?
Cr2 O3 Cr1 98.20(4) . . ?
C7 O3 Cr1 131.01(8) . . ?
C7 O3 Cr2 110.78(8) . . ?
Cr2 O4 H4 118.1(17) . . ?
C9 O4 Cr2 116.09(8) . . ?
C9 O4 H4 108.9(17) . . ?
C11 O5 Cr1 127.02(9) . . ?
C11 O6 Cr2 127.44(9) . . ?
C1 N1 Cr1 107.43(8) . . ?
C3 N1 Cr1 104.93(9) . . ?
C3 N1 C1 110.86(11) . . ?
C5 N1 Cr1 113.68(9) . . ?
C5 N1 C1 110.48(12) . . ?
C5 N1 C3 109.34(12) . . ?
C6 N2 Cr2 107.20(8) . . ?
C8 N2 Cr2 105.40(8) . . ?
C8 N2 C6 110.92(11) . . ?
C10 N2 Cr2 113.80(9) . . ?
C10 N2 C6 110.49(11) . . ?
C10 N2 C8 108.93(11) . . ?
N1 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
N1 C1 C2 109.35(11) . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
O1 C2 C1 106.16(11) . . ?
O1 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C1 C2 H2A 110.5 . . ?
C1 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
N1 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
N1 C3 C4 110.02(12) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
O2 C4 C3 107.89(12) . . ?
O2 C4 H4A 110.1 . . ?
O2 C4 H4B 110.1 . . ?
C3 C4 H4A 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
N2 C6 C7 109.97(11) . . ?
H6A C6 H6B 108.2 . . ?
C7 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
O3 C7 C6 106.99(11) . . ?
O3 C7 H7A 110.3 . . ?
O3 C7 H7B 110.3 . . ?
C6 C7 H7A 110.3 . . ?
C6 C7 H7B 110.3 . . ?
H7A C7 H7B 108.6 . . ?
N2 C8 H8A 109.7 . . ?
N2 C8 H8B 109.7 . . ?
N2 C8 C9 109.96(12) . . ?
H8A C8 H8B 108.2 . . ?
C9 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
O4 C9 C8 107.15(12) . . ?
O4 C9 H9A 110.3 . . ?
O4 C9 H9B 110.3 . . ?
C8 C9 H9A 110.3 . . ?
C8 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 O6 125.37(13) . . ?
O5 C11 C12 117.18(12) . . ?
O6 C11 C12 117.45(12) . . ?
C13 C12 C11 120.53(13) . . ?
C17 C12 C11 119.65(12) . . ?
C17 C12 C13 119.78(13) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.89(14) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 119.9 . . ?
C13 C14 C15 120.15(14) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 119.92(14) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.07(14) . . ?
C17 C16 H16 120.0 . . ?
C12 C17 H17 119.9 . . ?
C16 C17 C12 120.12(13) . . ?
C16 C17 H17 119.9 . . ?

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 H2 Cl3 0.76(2) 2.19(2) 2.9377(12) 170(2) .
O4 H4 Cl3 0.77(2) 2.17(2) 2.9388(11) 175(2) .

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 C2 C1 50.09(12) . . . . ?
Cr1 O2 C4 C3 23.24(15) . . . . ?
Cr1 O3 C7 C6 170.36(9) . . . . ?
Cr1 O5 C11 O6 -11.4(2) . . . . ?
Cr1 O5 C11 C12 167.93(9) . . . . ?
Cr1 N1 C1 C2 26.77(13) . . . . ?
Cr1 N1 C3 C4 45.32(13) . . . . ?
Cr2 O1 C2 C1 171.25(9) . . . . ?
Cr2 O3 C7 C6 48.21(13) . . . . ?
Cr2 O4 C9 C8 23.80(15) . . . . ?
Cr2 O6 C11 O5 1.7(2) . . . . ?
Cr2 O6 C11 C12 -177.61(8) . . . . ?
Cr2 N2 C6 C7 25.63(14) . . . . ?
Cr2 N2 C8 C9 45.73(13) . . . . ?
O5 C11 C12 C13 23.61(19) . . . . ?
O5 C11 C12 C17 -153.93(13) . . . . ?
O6 C11 C12 C13 -157.04(13) . . . . ?
O6 C11 C12 C17 25.41(19) . . . . ?
N1 C1 C2 O1 -49.79(14) . . . . ?
N1 C3 C4 O2 -45.71(16) . . . . ?
N2 C6 C7 O3 -48.02(16) . . . . ?
N2 C8 C9 O4 -45.90(16) . . . . ?
C1 N1 C3 C4 -70.36(15) . . . . ?
C3 N1 C1 C2 140.89(12) . . . . ?
C5 N1 C1 C2 -97.74(13) . . . . ?
C5 N1 C3 C4 167.61(13) . . . . ?
C6 N2 C8 C9 -69.97(15) . . . . ?
C8 N2 C6 C7 140.21(12) . . . . ?
C10 N2 C6 C7 -98.89(14) . . . . ?
C10 N2 C8 C9 168.21(12) . . . . ?
C11 C12 C13 C14 179.91(13) . . . . ?
C11 C12 C17 C16 178.58(13) . . . . ?
C12 C13 C14 C15 1.6(2) . . . . ?
C13 C12 C17 C16 1.0(2) . . . . ?
C13 C14 C15 C16 0.9(2) . . . . ?
C14 C15 C16 C17 -2.4(2) . . . . ?
C15 C16 C17 C12 1.5(2) . . . . ?
C17 C12 C13 C14 -2.5(2) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-24
_olex2_date_sample_submission    2016-11-24
_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 L145
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.806
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1579651'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-06-07 downloaded from the CCDC.
;
# local name eb16255


_audit_creation_date             2016-11-11
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H24 Cl4 Cr2 N2 O4'
_chemical_formula_sum            'C10 H24 Cl4 Cr2 N2 O4'
_chemical_formula_weight         482.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl'
_chemical_oxdiff_usercomment     '@ 120 K L48o'
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      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                   6.8880(2)
_cell_length_b                   9.9275(3)
_cell_length_c                   12.9510(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.457(3)
_cell_angle_gamma                90
_cell_volume                     882.91(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8165
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.3690
_cell_measurement_theta_min      3.7540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.851
_exptl_absorpt_correction_T_max  0.94411
_exptl_absorpt_correction_T_min  0.94411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43h (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             492
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 2 -7 0.1473
-9 -1 7 0.1285
-1 -11 -11 0.0506
1 11 11 0.0506
-1 -10 12 0.0049
1 10 -13 0.0623

_exptl_crystal_recrystallization_method 
'The material was recrystallised from acetonitrile by hydrothermal bomb'
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.069
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
8.9879 1.9903 -6.9928 -0.7462 0.4790 0.4336
-8.9878 -0.9917 6.9925 0.7409 -0.4246 -0.4794
-0.9998 -10.9910 -10.9816 0.3846 -0.2414 0.8915
0.9998 10.9910 10.9816 -0.3846 0.2414 -0.8915
-0.9997 -9.9780 11.9882 -0.0984 -0.9653 -0.0244
0.9996 9.9774 -12.9869 0.1191 0.9992 0.0622

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15425
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.807
_diffrn_reflns_theta_min         3.155
_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 0.999
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00  22.00   1.00    5.00    --   -9.43 -77.00-180.00  105
  2  ω    -20.00  30.00   1.00    5.00    --   -9.43 -99.00  30.00   50
  3  ω    -16.00  81.00   1.00    5.00    --   10.84  57.00  90.00   97
  4  ω    -16.00  81.00   1.00    5.00    --   10.84  57.00   0.00   97
  5  ω    -59.00  37.00   1.00    5.00    --   10.84 -57.00 -60.00   96
  6  ω    -20.00  51.00   1.00    5.00    --   10.84 -99.00  60.00   71
  7  ω    -20.00  16.00   1.00    5.00    --   10.84 -99.00 -90.00   36
  8  ω    -20.00  51.00   1.00    5.00    --   10.84 -99.00-180.00   71
;
_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      -0.0980290000
_diffrn_orient_matrix_UB_12      -0.0053016000
_diffrn_orient_matrix_UB_13      -0.0207922000
_diffrn_orient_matrix_UB_21      0.0148357000
_diffrn_orient_matrix_UB_22      0.0545039000
_diffrn_orient_matrix_UB_23      -0.0339229000
_diffrn_orient_matrix_UB_31      0.0289672000
_diffrn_orient_matrix_UB_32      -0.0459305000
_diffrn_orient_matrix_UB_33      -0.0378461000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2149
_reflns_number_total             2315
_reflns_odcompleteness_completeness 99.79
_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 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43h (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         0.378
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2315
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0250
_refine_ls_restrained_S_all      1.083
_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)+(0.0241P)²+0.4782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0576
_refine_special_details          
;
All H atoms were identified from a difference Fourier 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.         11 Note
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  Cl1     ..        5.5 s.u.
793_ALERT_4_G The Model has Chirality at N1      (Centro SPGR)          R Verify
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           1 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        208 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
978_ALERT_2_G Number C-C Bonds with Positive Residual Density           2 Note


Not significant


#===============================================================================
 
#===============================================================================
! Congratulations ! : No (A,B,C) ALERT Conditions were Detected - Check G-ALERTS
#===============================================================================
;
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_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 0.04684(3) 0.86235(2) 0.95870(2) 0.00820(8) Uani 1 1 d . . . . .
Cl1 Cl 0.17552(5) 0.95214(4) 0.81186(3) 0.01345(9) Uani 1 1 d . . . . .
Cl2 Cl -0.09610(6) 0.68850(4) 0.86392(3) 0.01462(10) Uani 1 1 d . . . . .
O1 O 0.16835(15) 1.00811(11) 1.04352(8) 0.0097(2) Uani 1 1 d . . . . .
O2 O -0.06698(16) 0.78471(12) 1.08660(9) 0.0118(2) Uani 1 1 d . . . . .
H2 H -0.107(3) 0.840(2) 1.1203(16) 0.019(5) Uiso 1 1 d . . . . .
N1 N 0.28937(19) 0.75016(13) 1.01970(10) 0.0108(3) Uani 1 1 d . . . . .
C1 C 0.3004(2) 0.96158(16) 1.12615(12) 0.0116(3) Uani 1 1 d . . . . .
H1A H 0.394(3) 1.0334(18) 1.1480(14) 0.009(4) Uiso 1 1 d . . . . .
H1B H 0.229(3) 0.9362(18) 1.1848(14) 0.007(4) Uiso 1 1 d . . . . .
C2 C 0.4166(2) 0.84634(16) 1.08409(12) 0.0123(3) Uani 1 1 d . . . . .
H2A H 0.503(3) 0.8819(18) 1.0410(13) 0.008(4) Uiso 1 1 d . . . . .
H2B H 0.491(3) 0.7977(19) 1.1394(14) 0.012(4) Uiso 1 1 d . . . . .
C3 C 0.0551(2) 0.69270(17) 1.15009(13) 0.0146(3) Uani 1 1 d . . . . .
H3A H -0.022(3) 0.6190(19) 1.1721(14) 0.010(4) Uiso 1 1 d . . . . .
H3B H 0.110(3) 0.7401(19) 1.2115(14) 0.013(4) Uiso 1 1 d . . . . .
C4 C 0.2091(2) 0.64090(16) 1.08317(13) 0.0138(3) Uani 1 1 d . . . . .
H4A H 0.152(3) 0.5728(18) 1.0349(14) 0.008(4) Uiso 1 1 d . . . . .
H4B H 0.312(3) 0.6024(19) 1.1255(14) 0.013(5) Uiso 1 1 d . . . . .
C5 C 0.4087(3) 0.68475(18) 0.94267(14) 0.0169(3) Uani 1 1 d . . . . .
H5A H 0.327(3) 0.624(2) 0.9044(15) 0.018(5) Uiso 1 1 d . . . . .
H5B H 0.517(3) 0.643(2) 0.9766(15) 0.017(5) Uiso 1 1 d . . . . .
H5C H 0.457(3) 0.751(2) 0.8971(16) 0.022(5) Uiso 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 2.3364(4) . ?
Cr1 Cl2 2.2950(4) . ?
Cr1 O1 1.9609(11) 3_577 ?
Cr1 O1 1.9642(11) . ?
Cr1 O2 2.0382(11) . ?
Cr1 N1 2.1095(13) . ?
O1 C1 1.4263(18) . ?
O2 H2 0.77(2) . ?
O2 C3 1.4526(19) . ?
N1 C2 1.504(2) . ?
N1 C4 1.493(2) . ?
N1 C5 1.490(2) . ?
C1 H1A 0.987(19) . ?
C1 H1B 0.970(18) . ?
C1 C2 1.521(2) . ?
C2 H2A 0.919(19) . ?
C2 H2B 0.976(19) . ?
C3 H3A 0.960(19) . ?
C3 H3B 0.975(19) . ?
C3 C4 1.511(2) . ?
C4 H4A 0.982(18) . ?
C4 H4B 0.94(2) . ?
C5 H5A 0.94(2) . ?
C5 H5B 0.93(2) . ?
C5 H5C 0.96(2) . ?

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 91.470(15) . . ?
O1 Cr1 Cl1 94.13(3) 3_577 . ?
O1 Cr1 Cl1 90.12(3) . . ?
O1 Cr1 Cl2 178.33(3) . . ?
O1 Cr1 Cl2 101.13(3) 3_577 . ?
O1 Cr1 O1 79.27(5) 3_577 . ?
O1 Cr1 O2 89.89(5) . . ?
O1 Cr1 O2 85.52(5) 3_577 . ?
O1 Cr1 N1 158.04(5) 3_577 . ?
O1 Cr1 N1 83.62(5) . . ?
O2 Cr1 Cl1 179.64(4) . . ?
O2 Cr1 Cl2 88.52(4) . . ?
O2 Cr1 N1 80.76(5) . . ?
N1 Cr1 Cl1 99.60(4) . . ?
N1 Cr1 Cl2 95.60(4) . . ?
Cr1 O1 Cr1 100.73(5) 3_577 . ?
C1 O1 Cr1 113.59(9) . . ?
C1 O1 Cr1 131.34(9) . 3_577 ?
Cr1 O2 H2 111.7(16) . . ?
C3 O2 Cr1 117.10(9) . . ?
C3 O2 H2 110.5(16) . . ?
C2 N1 Cr1 106.44(9) . . ?
C4 N1 Cr1 105.87(9) . . ?
C4 N1 C2 112.38(12) . . ?
C5 N1 Cr1 116.20(10) . . ?
C5 N1 C2 108.65(12) . . ?
C5 N1 C4 107.41(13) . . ?
O1 C1 H1A 110.1(11) . . ?
O1 C1 H1B 109.8(11) . . ?
O1 C1 C2 107.31(12) . . ?
H1A C1 H1B 108.8(14) . . ?
C2 C1 H1A 107.2(11) . . ?
C2 C1 H1B 113.5(11) . . ?
N1 C2 C1 112.07(12) . . ?
N1 C2 H2A 106.5(11) . . ?
N1 C2 H2B 110.1(11) . . ?
C1 C2 H2A 108.3(11) . . ?
C1 C2 H2B 111.7(11) . . ?
H2A C2 H2B 107.9(15) . . ?
O2 C3 H3A 109.8(11) . . ?
O2 C3 H3B 109.3(11) . . ?
O2 C3 C4 106.89(12) . . ?
H3A C3 H3B 108.3(15) . . ?
C4 C3 H3A 109.8(11) . . ?
C4 C3 H3B 112.7(11) . . ?
N1 C4 C3 112.02(13) . . ?
N1 C4 H4A 107.2(10) . . ?
N1 C4 H4B 108.8(12) . . ?
C3 C4 H4A 109.7(11) . . ?
C3 C4 H4B 109.4(12) . . ?
H4A C4 H4B 109.6(15) . . ?
N1 C5 H5A 107.2(12) . . ?
N1 C5 H5B 109.9(12) . . ?
N1 C5 H5C 110.5(12) . . ?
H5A C5 H5B 112.6(17) . . ?
H5A C5 H5C 109.6(17) . . ?
H5B C5 H5C 107.0(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 C1 C2 171.93(10) 3_577 . . . ?
Cr1 O1 C1 C2 41.03(14) . . . . ?
Cr1 O2 C3 C4 -19.84(16) . . . . ?
Cr1 N1 C2 C1 26.89(14) . . . . ?
Cr1 N1 C4 C3 -44.30(15) . . . . ?
O1 C1 C2 N1 -44.38(16) . . . . ?
O2 C3 C4 N1 42.43(17) . . . . ?
C2 N1 C4 C3 71.50(16) . . . . ?
C4 N1 C2 C1 -88.56(15) . . . . ?
C5 N1 C2 C1 152.72(13) . . . . ?
C5 N1 C4 C3 -169.06(14) . . . . ?

_shelx_SHELXL_version_number     2016/6
_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 L48o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.772


####


