# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1855222'
_audit_update_record             
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
# local name EB16234
_audit_creation_date             2017-03-03
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H72 Cr2 Mn5 N12 O12, 4(Cl1 O4), 10 C H4 O'
_chemical_formula_sum            'C82 H112 Cl4 Cr2 Mn5 N12 O38'
_chemical_formula_weight         2394.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Mn Cl Cr'
_chemical_oxdiff_usercomment     '@ 120 K 749o'
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'
Mn Mn -0.5299 2.8052 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   14.7045(6)
_cell_length_b                   14.7045(6)
_cell_length_c                   38.106(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7135.4(11)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    3738
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      50.1250
_cell_measurement_theta_min      4.1470
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.898
_exptl_absorpt_correction_T_max  0.8734
_exptl_absorpt_correction_T_min  0.2634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0991 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.3016.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3699
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 1 0.0821
0 -1 -1 0.0821
-5 5 4 0.0797
5 -5 -4 0.0797
5 0 1 0.0677
-1 0 0 0.0887
0 0 1 0.0119
0 0 -1 0.0119

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.024
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 1.0002 1.0048 0.0037 -0.0469 0.1186
0.0002 -1.0002 -1.0048 -0.0037 0.0469 -0.1186
-5.0026 4.9947 4.0358 -0.0172 0.3649 0.5084
5.0026 -4.9947 -4.0358 0.0172 -0.3649 -0.5084
5.0016 0.0065 0.9882 0.0355 -0.5995 0.0844
-1.0002 -0.0014 0.0023 -0.0147 0.1193 -0.0141
0.0003 -0.0003 0.9996 -0.0379 -0.0030 0.0139
-0.0003 0.0003 -0.9996 0.0379 0.0030 -0.0139

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            17837
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        50.499
_diffrn_reflns_theta_max         50.499
_diffrn_reflns_theta_min         3.479
_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 0.3322
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  -2.00   1.00   10.00    --  -43.17 125.00  30.00   94
  2  ω   -130.00  43.00   1.00   10.00    --  -43.17   0.00  60.00  173
  3  ω    -66.00  29.00   1.00   10.00    --  -43.17  38.00 -60.00   95
  4  ω     23.00  98.00   1.00   10.00    --   43.17-125.00-120.00   75
  5  ω     23.00  98.00   1.00   10.00    --   43.17-125.00  60.00   75
  6  ω     40.00 135.00   1.00   30.00    --  111.00 -45.00 -30.00   95
  7  ω     41.00 139.00   1.00   30.00    --  111.00 -61.00  90.00   98
  8  ω     37.00 142.00   1.00   30.00    --  111.00 -77.00-150.00  105
  9  ω     36.00 135.00   1.00   30.00    --  111.00 -30.00-150.00   99
 10  ω     87.00 178.00   1.00   30.00    --  111.00  30.00 -90.00   91
 11  ω     80.00 178.00   1.00   30.00    --  111.00  77.00-150.00   98
 12  ω     94.00 178.00   1.00   30.00    --  111.00 125.00 -90.00   84
 13  ω     39.00 121.00   1.00   30.00    --  111.00-125.00  30.00   82
 14  ω     87.00 178.00   1.00   30.00    --  111.00  30.00-180.00   91
 15  ω     39.00 121.00   1.00   30.00    --  111.00-125.00-150.00   82
 16  ω     94.00 178.00   1.00   30.00    --  111.00 125.00 150.00   84
 17  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00  60.00   79
 18  ω   -113.00 -17.00   1.00   10.00    --  -43.17 -57.00-120.00   96
 19  ω   -117.00 -12.00   1.00   10.00    --  -43.17 -77.00  90.00  105
 20  ω   -113.00 -17.00   1.00   10.00    --  -43.17 -57.00 -30.00   96
;
_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      0.0145418000
_diffrn_orient_matrix_UB_12      0.0417511000
_diffrn_orient_matrix_UB_13      -0.0379047000
_diffrn_orient_matrix_UB_21      -0.1192148000
_diffrn_orient_matrix_UB_22      -0.0439265000
_diffrn_orient_matrix_UB_23      -0.0030012000
_diffrn_orient_matrix_UB_31      0.0139978000
_diffrn_orient_matrix_UB_32      0.1045978000
_diffrn_orient_matrix_UB_33      0.0138866000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1482
_reflns_number_total             1673
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         1673
_refine_ls_number_restraints     137
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0737
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1734P)²+32.5148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2045
_refine_ls_wR_factor_ref         0.2110
_refine_special_details          
;
The diffraction pattern was found to be affected by twinning, handled with twin law [-1 -1 0 / 0 1 0/ 0 0 -1] and refined twin scale factor 0.228(4).  The measured data set was very weak, and the resolution was cut at 1 A.  The SQUEEZE routine of PLATON was used to handle electron density corresponding with exactly ten molecules of methanol per asymmetric unit, which could not be modelled using discrete atoms.  This missing solvent is included in the total formula, triggering checkCIF alerts which should be ignored.

One ligand was modelled as disordered over two sites, consistent with very large ellipsoids.  Geometric and displacement ellipsoid restraints were used.

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      50.50 Degree

Discussed above

430_ALERT_2_A Short Inter D...A Contact  O1     ..  O2A     ..       2.36 Ang.

Consequence of ligand disorder.  The O atoms both bridge two metal centres.

#===============================================================================
088_ALERT_3_B Poor Data / Parameter Ratio ....................       6.43 Note

Noted above

341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............      0.034 Ang.

Consequence of weak data

430_ALERT_2_B Short Inter D...A Contact  O1     ..  O2      ..       2.69 Ang.
430_ALERT_2_B Short Inter D...A Contact  O2A    ..  N1      ..       2.79 Ang.
430_ALERT_2_B Short Inter D...A Contact  N1     ..  O2      ..       2.79 Ang.

Consequence of disorder.

#===============================================================================
018_ALERT_1_C _diffrn_measured_fraction_theta_max .NE. *_full           ! Check
214_ALERT_2_C Atom O2A     (Anion/Solvent) ADP max/min Ratio          4.2 prolat
214_ALERT_2_C Atom C11A    (Anion/Solvent) ADP max/min Ratio          4.8 oblate
234_ALERT_4_C Large Hirshfeld Difference Mn1    --  N1      ..       0.16 Ang.
234_ALERT_4_C Large Hirshfeld Difference Cr1    --  N1      ..       0.16 Ang.
234_ALERT_4_C Large Hirshfeld Difference O1     --  C6      ..       0.23 Ang.
234_ALERT_4_C Large Hirshfeld Difference C3     --  C4      ..       0.22 Ang.
234_ALERT_4_C Large Hirshfeld Difference C5     --  C6      ..       0.19 Ang.
241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         C3 Check
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.4 Note
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.5 Note
309_ALERT_2_C Single Bonded Oxygen (C-O > 1.3 Ang) ...........        O2A Check
309_ALERT_2_C Single Bonded Oxygen (C-O > 1.3 Ang) ...........         O2 Check

The above are noted.  Geometric restraints were used where applicable.  This model is based on rather poor data.

#===============================================================================
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.712(4)
 0.288(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Shared sites
{Mn1, Cr1}
4. Uiso/Uaniso restraints and constraints
Uanis(Mn1) = Uanis(Cr1)
5. Rigid body (RIGU) restrains
 Cl2, Cl2, Cl2, O5, O5, O6, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, Cl1, Cl1, O4, O4, O3, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2A, N2A, C7A, C12A, C11A, C8A, C10A, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, N2, C7, C12, C11, C8, C10, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O2, N2, C7, C12, C11, C8, C10, C9} sigma for 1-2: 0.02, 1-3: 0.02
as
{O2A, N2A, C7A, C12A, C11A, C8A, C10A, C9A}
7. Others
 Sof(O2A)=Sof(N2A)=Sof(C7A)=Sof(H7A)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C11A)=
 Sof(C8A)=Sof(H8A)=Sof(C10A)=Sof(H10A)=Sof(C9A)=Sof(H9A)=1-FVAR(1)
 Sof(O2)=Sof(N2)=Sof(C7)=Sof(H7)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(C8)=
 Sof(H8)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=FVAR(1)
 Fixed Sof: Mn1(0.66666) Cr1(0.33333)
8.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C12A(H12C,H12D), C6(H6A,H6B)
8.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C9(H9), C7A(H7A), C8A(H8A), C10A(H10A), C9A(H9A),
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Mn1 Mn 0.48373(14) 0.39429(14) 0.33706(5) 0.0685(8) Uani 0.6667 1 d . . . A 1
O2 O 0.3979(17) 0.2591(19) 0.3614(9) 0.035(8) Uani 0.46(7) 1 d D U . A 1
N2 N 0.301(4) 0.053(2) 0.3704(13) 0.062(9) Uani 0.46(7) 1 d D U . A 1
C7 C 0.259(4) -0.053(2) 0.3722(13) 0.073(10) Uani 0.46(7) 1 d D U . A 1
H7 H 0.279110 -0.087618 0.355422 0.088 Uiso 0.46(7) 1 calc R . . A 1
C12 C 0.318(4) 0.218(3) 0.3878(14) 0.077(14) Uani 0.46(7) 1 d D U . A 1
H12A H 0.264451 0.237040 0.382128 0.093 Uiso 0.46(7) 1 calc R . . A 1
H12B H 0.349826 0.249537 0.410669 0.093 Uiso 0.46(7) 1 calc R . . A 1
C11 C 0.265(4) 0.097(2) 0.3907(12) 0.063(10) Uani 0.46(7) 1 d D U . A 1
C8 C 0.188(4) -0.111(3) 0.3984(13) 0.098(14) Uani 0.46(7) 1 d D U . A 1
H8 H 0.161720 -0.183943 0.400589 0.118 Uiso 0.46(7) 1 calc R . . A 1
C10 C 0.192(4) 0.042(3) 0.4157(15) 0.098(13) Uani 0.46(7) 1 d D U . A 1
H10 H 0.165302 0.074468 0.430537 0.117 Uiso 0.46(7) 1 calc R . . A 1
C9 C 0.159(3) -0.065(3) 0.4190(12) 0.099(13) Uani 0.46(7) 1 d D U . A 1
H9 H 0.112811 -0.103298 0.437552 0.119 Uiso 0.46(7) 1 calc R . . A 1
Mn2 Mn 0.666667 0.333333 0.333333 0.0558(11) Uani 1 6 d S T P A .
Cr1 Cr 0.48373(14) 0.39429(14) 0.33706(5) 0.0685(8) Uani 0.3333 1 d . . . A 2
O2A O 0.393(2) 0.2431(19) 0.3492(10) 0.072(8) Uani 0.54(7) 1 d D U . A 2
N2A N 0.318(3) 0.0433(18) 0.3611(12) 0.062(7) Uani 0.54(7) 1 d D U . A 2
C7A C 0.290(4) -0.0595(19) 0.3634(12) 0.094(11) Uani 0.54(7) 1 d D U . A 2
H7A H 0.316168 -0.088737 0.346750 0.113 Uiso 0.54(7) 1 calc R . . A 2
C12A C 0.317(3) 0.199(2) 0.3774(13) 0.088(10) Uani 0.54(7) 1 d D U . A 2
H12C H 0.255031 0.206809 0.371639 0.106 Uiso 0.54(7) 1 calc R . . A 2
H12D H 0.348147 0.238491 0.399317 0.106 Uiso 0.54(7) 1 calc R . . A 2
C11A C 0.280(3) 0.082(2) 0.3831(11) 0.082(10) Uani 0.54(7) 1 d D U . A 2
C8A C 0.223(4) -0.123(2) 0.3898(13) 0.114(12) Uani 0.54(7) 1 d D U . A 2
H8A H 0.203783 -0.194675 0.391396 0.137 Uiso 0.54(7) 1 calc R . . A 2
C10A C 0.207(4) 0.019(3) 0.4066(15) 0.109(11) Uani 0.54(7) 1 d D U . A 2
H10A H 0.167769 0.043264 0.419622 0.131 Uiso 0.54(7) 1 calc R . . A 2
C9A C 0.190(5) -0.083(3) 0.4112(14) 0.15(2) Uani 0.54(7) 1 d D U . A 2
H9A H 0.152107 -0.122031 0.431215 0.182 Uiso 0.54(7) 1 calc R . . A 2
O1 O 0.6294(7) 0.4391(6) 0.3610(2) 0.074(2) Uani 1 1 d . . . . .
N1 N 0.4702(10) 0.4667(8) 0.3815(4) 0.099(4) Uani 1 1 d . . . . .
C1 C 0.4082(13) 0.5029(13) 0.3877(6) 0.115(6) Uani 1 1 d . . . . .
H1 H 0.360857 0.496626 0.369626 0.139 Uiso 1 1 calc R . . . .
C2 C 0.4059(17) 0.5494(19) 0.4182(7) 0.145(8) Uani 1 1 d . . . . .
H2 H 0.357061 0.573223 0.421178 0.174 Uiso 1 1 calc R . . . .
C3 C 0.477(2) 0.5622(18) 0.4457(7) 0.160(8) Uani 1 1 d . . . . .
H3 H 0.473234 0.590308 0.467774 0.192 Uiso 1 1 calc R . . . .
C4 C 0.5530(19) 0.5321(14) 0.4395(5) 0.138(7) Uani 1 1 d . . . . .
H4 H 0.604762 0.543085 0.456499 0.165 Uiso 1 1 calc R . . . .
C5 C 0.5481(15) 0.4851(11) 0.4069(5) 0.109(5) Uani 1 1 d . . . . .
C6 C 0.6283(12) 0.4509(12) 0.3981(4) 0.099(5) Uani 1 1 d . . . . .
H6A H 0.698856 0.504392 0.406405 0.119 Uiso 1 1 calc R . . . .
H6B H 0.608658 0.383504 0.409860 0.119 Uiso 1 1 calc R . . . .
Cl1 Cl 0.666667 0.333333 0.4887(2) 0.142(3) Uani 1 3 d S TU P . .
O3 O 0.5679(16) 0.316(2) 0.4756(5) 0.274(14) Uani 1 1 d . U . . .
O4 O 0.666667 0.333333 0.5252(6) 0.181(11) Uani 1 3 d S TU P . .
Cl2 Cl 0.333333 0.666667 0.3309(2) 0.112(2) Uani 1 3 d S TU P . .
O5 O 0.2653(10) 0.5644(9) 0.3344(4) 0.154(5) Uani 1 1 d . U . . .
O6 O 0.333333 0.666667 0.2918(9) 0.235(15) Uani 1 3 d S TU 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
Mn1 O2 1.974(17) . ?
Mn1 O2 2.18(3) 17 ?
Mn1 N2 2.26(3) 17 ?
Mn1 O1 2.107(8) . ?
Mn1 O1 2.170(8) 18_545 ?
Mn1 N1 2.063(13) . ?
O2 C12 1.43(2) . ?
N2 C7 1.36(2) . ?
N2 C11 1.28(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.39(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.55(3) . ?
C11 C10 1.36(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.24(4) . ?
C10 H10 0.9500 . ?
C10 C9 1.39(4) . ?
C9 H9 0.9500 . ?
Mn2 O1 2.163(8) 2_655 ?
Mn2 O1 2.163(8) 18_545 ?
Mn2 O1 2.163(8) . ?
Mn2 O1 2.163(8) 17 ?
Mn2 O1 2.163(8) 16_655 ?
Mn2 O1 2.163(8) 3_665 ?
Cr1 O2A 1.79(3) 17 ?
Cr1 O2A 1.99(2) . ?
Cr1 N2A 1.96(3) 17 ?
Cr1 O1 2.170(8) 18_545 ?
Cr1 O1 2.107(8) . ?
Cr1 N1 2.063(13) . ?
O2A C12A 1.45(2) . ?
N2A C7A 1.35(2) . ?
N2A C11A 1.29(3) . ?
C7A H7A 0.9500 . ?
C7A C8A 1.39(3) . ?
C12A H12C 0.9900 . ?
C12A H12D 0.9900 . ?
C12A C11A 1.55(3) . ?
C11A C10A 1.35(3) . ?
C8A H8A 0.9500 . ?
C8A C9A 1.24(4) . ?
C10A H10A 0.9500 . ?
C10A C9A 1.40(4) . ?
C9A H9A 0.9500 . ?
O1 C6 1.427(17) . ?
N1 C1 1.285(19) . ?
N1 C5 1.42(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.36(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.42(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.41(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.41(2) . ?
C5 C6 1.53(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
Cl1 O3 1.436(19) . ?
Cl1 O3 1.436(19) 3_665 ?
Cl1 O3 1.436(18) 2_655 ?
Cl1 O4 1.39(2) . ?
Cl2 O5 1.332(12) 3_565 ?
Cl2 O5 1.332(12) 2_665 ?
Cl2 O5 1.332(12) . ?
Cl2 O6 1.49(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mn1 O2 168.9(12) . 17 ?
O2 Mn1 N2 73.3(11) 17 17 ?
O2 Mn1 N2 110.2(16) . 17 ?
O2 Mn1 O1 98.6(9) . . ?
O2 Mn1 O1 80.7(10) . 18_545 ?
O2 Mn1 N1 87.5(11) . . ?
O1 Mn1 O2 88.4(9) 18_545 17 ?
O1 Mn1 O2 77.6(5) . 17 ?
O1 Mn1 N2 97.5(15) 18_545 17 ?
O1 Mn1 N2 150.9(10) . 17 ?
O1 Mn1 O1 82.8(4) . 18_545 ?
N1 Mn1 O2 102.0(9) . 17 ?
N1 Mn1 N2 104.5(15) . 17 ?
N1 Mn1 O1 80.2(5) . . ?
N1 Mn1 O1 157.5(4) . 18_545 ?
Mn1 O2 Mn1 102.7(12) . 18_545 ?
C12 O2 Mn1 137.4(17) . . ?
C12 O2 Mn1 118.7(13) . 18_545 ?
C7 N2 Mn1 121(2) . 18_545 ?
C11 N2 Mn1 119.4(15) . 18_545 ?
C11 N2 C7 119(2) . . ?
N2 C7 H7 119.8 . . ?
N2 C7 C8 120(3) . . ?
C8 C7 H7 119.8 . . ?
O2 C12 H12A 109.2 . . ?
O2 C12 H12B 109.2 . . ?
O2 C12 C11 112.2(18) . . ?
H12A C12 H12B 107.9 . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
N2 C11 C12 115.8(18) . . ?
N2 C11 C10 122(2) . . ?
C10 C11 C12 122(3) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 119(3) . . ?
C9 C8 H8 120.6 . . ?
C11 C10 H10 121.2 . . ?
C11 C10 C9 118(3) . . ?
C9 C10 H10 121.2 . . ?
C8 C9 C10 122(3) . . ?
C8 C9 H9 118.9 . . ?
C10 C9 H9 118.9 . . ?
O1 Mn2 O1 180.0 18_545 3_665 ?
O1 Mn2 O1 81.7(3) 16_655 2_655 ?
O1 Mn2 O1 98.3(3) 16_655 17 ?
O1 Mn2 O1 98.3(3) 3_665 . ?
O1 Mn2 O1 180.0 17 2_655 ?
O1 Mn2 O1 81.7(3) 17 3_665 ?
O1 Mn2 O1 98.3(3) 2_655 . ?
O1 Mn2 O1 180.0 16_655 . ?
O1 Mn2 O1 81.7(3) 16_655 3_665 ?
O1 Mn2 O1 81.7(3) 17 . ?
O1 Mn2 O1 98.3(3) 3_665 2_655 ?
O1 Mn2 O1 81.7(3) 18_545 . ?
O1 Mn2 O1 98.3(3) 16_655 18_545 ?
O1 Mn2 O1 81.7(3) 18_545 2_655 ?
O1 Mn2 O1 98.3(3) 17 18_545 ?
O2A Cr1 O2A 165.5(12) 17 . ?
O2A Cr1 O1 105.0(10) . . ?
O2A Cr1 O1 73.9(9) 17 . ?
O2A Cr1 N1 101.6(11) . . ?
O2A Cr1 N1 92.5(12) 17 . ?
N2A Cr1 O2A 92.0(16) 17 . ?
N2A Cr1 O1 161.8(9) 17 . ?
N2A Cr1 N1 103.3(16) 17 . ?
O1 Cr1 O1 82.8(4) . 18_545 ?
N1 Cr1 O1 157.5(4) . 18_545 ?
N1 Cr1 O1 80.2(5) . . ?
C12A O2A Cr1 127.4(16) . . ?
C11A N2A C7A 119(2) . . ?
N2A C7A H7A 119.5 . . ?
N2A C7A C8A 121(3) . . ?
C8A C7A H7A 119.5 . . ?
O2A C12A H12C 109.4 . . ?
O2A C12A H12D 109.4 . . ?
O2A C12A C11A 111.2(18) . . ?
H12C C12A H12D 108.0 . . ?
C11A C12A H12C 109.4 . . ?
C11A C12A H12D 109.4 . . ?
N2A C11A C12A 114.4(18) . . ?
N2A C11A C10A 121(2) . . ?
C10A C11A C12A 125(2) . . ?
C7A C8A H8A 120.9 . . ?
C9A C8A C7A 118(3) . . ?
C9A C8A H8A 120.9 . . ?
C11A C10A H10A 121.2 . . ?
C11A C10A C9A 118(3) . . ?
C9A C10A H10A 121.2 . . ?
C8A C9A C10A 122(3) . . ?
C8A C9A H9A 119.2 . . ?
C10A C9A H9A 119.2 . . ?
Mn1 O1 Mn1 98.7(3) . 17 ?
Mn1 O1 Mn2 98.5(3) . . ?
Mn2 O1 Mn1 96.6(3) . 17 ?
Cr1 O1 Mn2 98.5(3) . . ?
C6 O1 Mn1 118.4(8) . 17 ?
C6 O1 Mn1 113.3(8) . . ?
C6 O1 Mn2 126.3(7) . . ?
C6 O1 Cr1 113.3(8) . . ?
C1 N1 Mn1 129.4(14) . . ?
C1 N1 Cr1 129.4(14) . . ?
C1 N1 C5 118.0(15) . . ?
C5 N1 Mn1 112.4(10) . . ?
C5 N1 Cr1 112.4(10) . . ?
N1 C1 H1 117.8 . . ?
N1 C1 C2 124(2) . . ?
C2 C1 H1 117.8 . . ?
C1 C2 H2 120.2 . . ?
C1 C2 C3 119.7(18) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.6(19) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 121.7 . . ?
C5 C4 C3 117(2) . . ?
C5 C4 H4 121.7 . . ?
N1 C5 C6 118.0(14) . . ?
C4 C5 N1 122.2(17) . . ?
C4 C5 C6 119.7(18) . . ?
O1 C6 C5 108.3(12) . . ?
O1 C6 H6A 110.0 . . ?
O1 C6 H6B 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
O3 Cl1 O3 108.5(9) 3_665 . ?
O3 Cl1 O3 108.5(10) 2_655 . ?
O3 Cl1 O3 108.5(9) 2_655 3_665 ?
O4 Cl1 O3 110.4(9) . . ?
O4 Cl1 O3 110.4(9) . 3_665 ?
O4 Cl1 O3 110.4(9) . 2_655 ?
O5 Cl2 O5 119.0(3) 3_565 . ?
O5 Cl2 O5 119.0(3) 3_565 2_665 ?
O5 Cl2 O5 119.0(3) . 2_665 ?
O5 Cl2 O6 95.7(9) 3_565 . ?
O5 Cl2 O6 95.7(9) 2_665 . ?
O5 Cl2 O6 95.7(9) . . ?

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
Mn1 O2 C12 C11 3(5) 18_545 . . . ?
Mn1 O2 C12 C11 169(4) . . . . ?
Mn1 N2 C7 C8 177(4) 18_545 . . . ?
Mn1 N2 C11 C12 -6(6) 18_545 . . . ?
Mn1 N2 C11 C10 -180(5) 18_545 . . . ?
Mn1 O1 C6 C5 84.9(12) 17 . . . ?
Mn1 O1 C6 C5 -29.9(13) . . . . ?
Mn1 N1 C1 C2 179.9(16) . . . . ?
Mn1 N1 C5 C4 -179.0(13) . . . . ?
Mn1 N1 C5 C6 0.4(16) . . . . ?
O2 C12 C11 N2 2(7) . . . . ?
O2 C12 C11 C10 175(5) . . . . ?
N2 C7 C8 C9 4(7) . . . . ?
N2 C11 C10 C9 1(8) . . . . ?
C7 N2 C11 C12 179(5) . . . . ?
C7 N2 C11 C10 5(8) . . . . ?
C7 C8 C9 C10 3(7) . . . . ?
C12 C11 C10 C9 -172(5) . . . . ?
C11 N2 C7 C8 -8(7) . . . . ?
C11 C10 C9 C8 -5(8) . . . . ?
Mn2 O1 C6 C5 -151.1(8) . . . . ?
Cr1 O2A C12A C11A -168(3) . . . . ?
Cr1 O1 C6 C5 -29.9(13) . . . . ?
Cr1 N1 C1 C2 179.9(16) . . . . ?
Cr1 N1 C5 C4 -179.0(13) . . . . ?
Cr1 N1 C5 C6 0.4(16) . . . . ?
O2A C12A C11A N2A -4(5) . . . . ?
O2A C12A C11A C10A -177(4) . . . . ?
N2A C7A C8A C9A 0(7) . . . . ?
N2A C11A C10A C9A 13(7) . . . . ?
C7A N2A C11A C12A -179(4) . . . . ?
C7A N2A C11A C10A -5(7) . . . . ?
C7A C8A C9A C10A 8(9) . . . . ?
C12A C11A C10A C9A -174(5) . . . . ?
C11A N2A C7A C8A -2(7) . . . . ?
C11A C10A C9A C8A -15(9) . . . . ?
N1 C1 C2 C3 1(3) . . . . ?
N1 C5 C6 O1 19.6(18) . . . . ?
C1 N1 C5 C4 6(2) . . . . ?
C1 N1 C5 C6 -174.5(14) . . . . ?
C1 C2 C3 C4 4(4) . . . . ?
C2 C3 C4 C5 -4(3) . . . . ?
C3 C4 C5 N1 -1(3) . . . . ?
C3 C4 C5 C6 179.6(16) . . . . ?
C4 C5 C6 O1 -161.0(15) . . . . ?
C5 N1 C1 C2 -6(3) . . . . ?

_platon_squeeze_details          '10 MeOH per wheel'
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 0.167 487 160 ' '
2 0.000 0.000 0.500 485 160 ' '
3 -0.333 0.333 0.833 490 160 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_date_sample_data_collection 2016-10-05
_olex2_date_sample_submission    2016-10-05
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id 749o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 2.330
_oxdiff_exptl_absorpt_empirical_full_min 0.624
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.712(4)
2 0.288(4)

_vrf_PLAT023_3                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      50.50 Degree
RESPONSE: Please see the _refine_special_details section of the CIF.
;
_vrf_PLAT430_3                   
;
PROBLEM: Short Inter D...A Contact  O1     ..  O2A     ..       2.36 Ang.
RESPONSE: Please see the _refine_special_details section of the CIF.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1855225'
_audit_update_record             
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT082_4                   
;
PROBLEM: High R1 Value ..................................       0.21 Report
RESPONSE:  Please see the _refine_special_details section of the CIF. 
;
_vrf_PLAT084_4                   
;
PROBLEM: High wR2 Value (i.e. &gt; 0.25) ...................       0.55 Report
RESPONSE:  Please see the _refine_special_details section of the CIF. 
;
_vrf_PLAT201_4                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         41 Report
RESPONSE:  Please see the _refine_special_details section of the CIF. 
;
_vrf_PLAT602_4                   
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info
RESPONSE: Please see the _refine_special_details section of the CIF.
;
# Added during the CSD deposition process: Wednesday 11 July 2018 03:04 PM
# end Validation Reply Form

# local name eb16230
_audit_creation_date             2018-02-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H72 Cr2 Cu5 N12 O12, 2(Cl O4), 2(N O3)'
_chemical_formula_sum            'C72 H72 Cl2 Cr2 Cu5 N14 O26'
_chemical_formula_weight         2042.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cu Cl Cr'
_chemical_oxdiff_usercomment     '@ 120 K 719o'
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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   14.5052(12)
_cell_length_b                   25.0735(19)
_cell_length_c                   25.095(5)
_cell_angle_alpha                90
_cell_angle_beta                 90.268(13)
_cell_angle_gamma                90
_cell_volume                     9127(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2785
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.7110
_cell_measurement_theta_min      4.9380
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.351
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4148
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
8 -8 4 0.0742
-8 8 -4 0.1009
0 -16 -2 0.0806
-8 -8 -6 0.0880
8 8 6 0.0667
-1 -1 10 0.0132
1 1 -10 0.0132
0 16 2 0.1180

_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.161
_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
8.0155 -7.9622 3.9371 -0.2865 0.8347 0.4984
-8.0155 7.9622 -3.9371 0.2865 -0.8347 -0.4984
0.0120 -15.9806 -1.9970 0.0169 -0.0414 0.9891
-8.0035 -8.0185 -5.9341 0.3034 -0.8761 0.4907
8.0035 8.0185 5.9341 -0.3034 0.8761 -0.4907
-0.9973 -1.0014 9.9954 -0.6171 -0.0968 -0.0076
0.9973 1.0014 -9.9954 0.6171 0.0968 0.0076
-0.0120 15.9806 1.9970 -0.0169 0.0414 -0.9891

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18466
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.751
_diffrn_reflns_theta_min         3.520
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00  31.00   1.00   10.00    --  -43.17  77.00 -30.00  106
  2  ω    -70.00  27.00   1.00   10.00    --  -43.17  57.00  90.00   97
  3  ω   -117.00 -12.00   1.00   10.00    --  -43.17 -77.00  30.00  105
  4  ω     83.00 178.00   1.00   30.00    --  111.00  61.00 -90.00   95
  5  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00-150.00   79
  6  ω     94.00 178.00   1.00   30.00    --  111.00 125.00  60.00   84
  7  ω     87.00 178.00   1.00   30.00    --  111.00  45.00 -30.00   91
  8  ω   -113.00 -56.00   1.00   10.00    --  -43.17 -57.00-150.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0007490000
_diffrn_orient_matrix_UB_12      0.0065664000
_diffrn_orient_matrix_UB_13      -0.0610059000
_diffrn_orient_matrix_UB_21      0.1060858000
_diffrn_orient_matrix_UB_22      0.0025256000
_diffrn_orient_matrix_UB_23      0.0011509000
_diffrn_orient_matrix_UB_31      0.0046520000
_diffrn_orient_matrix_UB_32      -0.0610871000
_diffrn_orient_matrix_UB_33      -0.0064155000
_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_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6177
_reflns_number_total             18466
_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 1.171.38.46 (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    ?
_refine_diff_density_max         4.515
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.346
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.446
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         18466
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.3043
_refine_ls_R_factor_gt           0.2142
_refine_ls_restrained_S_all      1.451
_refine_ls_shift/su_max          0.117
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5029
_refine_ls_wR_factor_ref         0.5502
_refine_special_details          
;
 Refined as a 3-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.563(5)
 0.126(3) 0.311(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C12-C11 = C6-C5 = C18-C17 = C36-C35 = C30-C29 = C24-C23
 1.51 with sigma of 0.02
 O1-C6 = O2-C12 = O6-C36 = O5-C30 = O3-C18 = O4-C24
 1.41 with sigma of 0.02
 Cl1-O9 = Cl1-O8 = Cl1-O10 = Cl1-O7
 1.41 with sigma of 0.02
 O11-N7 = O12-N7 = O13-N8 = O14-N8
 1.24 with sigma of 0.02
 O9-O8 = O10-O7
 2.28 with sigma of 0.04
 O9-O10 = O8-O7
 2.28 with sigma of 0.04
 O10-O8 = O9-O7
 2.28 with sigma of 0.04
 O14-O13 = O12-O11
 2.14 with sigma of 0.04
4. Others
 Fixed Uiso: C34(0.23954)
5.a Everything fixed:
 N8, O14, O13, N7, O12, O11
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30A,H30B),
 C36(H36A,H36B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C9(H9), C8(H8), C7(H7), C13(H13),
 C14(H14), C15(H15), C16(H16), C22(H22), C21(H21), C20(H20), C19(H19), C28(H28),
  C27(H27), C26(H26), C25(H25), C34(H34), C33(H33), C32(H32), C31(H31)
5.d Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N2(C11,C10,C9,C8,C7), N3(C13,C14,C15,C16,C17), N4(C23,C22,
 C21,C20,C19), N5(C29,C28,C27,C26,C25), N6(C35,C34,C33,C32,C31)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.750000 0.250000 0.250000 0.0753(18) Uani 1 2 d S T P . .
Cu2 Cu 0.5997(2) 0.34106(13) 0.25777(15) 0.0545(9) Uani 1 1 d . . . . .
Cu3 Cu 0.8102(3) 0.37080(15) 0.24369(18) 0.0787(13) Uani 1 1 d . . . . .
Cr1 Cr 0.5363(3) 0.22067(16) 0.2461(2) 0.0716(13) Uani 1 1 d . . . . .
O2 O 0.6537(12) 0.2046(7) 0.2095(8) 0.087(6) Uani 1 1 d D . . . .
O1 O 0.5972(6) 0.1604(4) 0.2599(4) 0.0119(16) Uiso 1 1 d D . . . .
O3 O 0.6309(11) 0.2783(7) 0.2973(10) 0.101(7) Uani 1 1 d D . . . .
O4 O 0.5174(9) 0.2903(5) 0.2231(5) 0.037(3) Uiso 1 1 d D . . . .
O5 O 0.7019(10) 0.3843(6) 0.2802(5) 0.052(4) Uiso 1 1 d D . . . .
O6 O 0.7335(17) 0.3185(6) 0.2050(8) 0.122(9) Uani 1 1 d D . . . .
N1 N 0.4347(9) 0.2183(6) 0.2952(6) 0.068(6) Uani 1 1 d . . . . .
C1 C 0.3604(11) 0.2531(5) 0.2985(7) 0.067(8) Uiso 1 1 d G . . . .
H1 H 0.355049 0.281242 0.274541 0.081 Uiso 1 1 calc R . . . .
C2 C 0.2942(10) 0.2459(6) 0.3377(8) 0.074(9) Uiso 1 1 d G . . . .
H2 H 0.244452 0.269232 0.339939 0.089 Uiso 1 1 calc R . . . .
C3 C 0.3022(11) 0.2039(7) 0.3735(6) 0.088(8) Uiso 1 1 d G . . . .
H3 H 0.257849 0.199077 0.399753 0.105 Uiso 1 1 calc R . . . .
C4 C 0.3765(12) 0.1691(6) 0.3702(6) 0.084(8) Uiso 1 1 d G . . . .
H4 H 0.381842 0.140930 0.394168 0.101 Uiso 1 1 calc R . . . .
C5 C 0.4427(10) 0.1762(6) 0.3310(6) 0.073(7) Uiso 1 1 d DG . . . .
N2 N 0.4831(14) 0.1904(8) 0.1767(6) 0.069(6) Uiso 1 1 d . . . . .
C11 C 0.5440(11) 0.1891(9) 0.1341(9) 0.21(2) Uiso 1 1 d DG . . . .
C10 C 0.5174(16) 0.1659(10) 0.0862(7) 0.114(11) Uiso 1 1 d G . . . .
H10 H 0.558194 0.165017 0.057709 0.137 Uiso 1 1 calc R . . . .
C9 C 0.4299(18) 0.1439(9) 0.0808(7) 0.155(16) Uiso 1 1 d G . . . .
H9 H 0.412119 0.128325 0.048715 0.186 Uiso 1 1 calc R . . . .
C8 C 0.3690(13) 0.1451(9) 0.1234(10) 0.125(13) Uiso 1 1 d G . . . .
H8 H 0.310400 0.130441 0.119752 0.150 Uiso 1 1 calc R . . . .
C7 C 0.3955(13) 0.1684(9) 0.1713(8) 0.139(14) Uiso 1 1 d G . . . .
H7 H 0.354755 0.169249 0.199784 0.167 Uiso 1 1 calc R . . . .
N3 N 0.5111(14) 0.3472(9) 0.3210(8) 0.109(10) Uani 1 1 d . . . . .
C13 C 0.4358(18) 0.3814(10) 0.3236(10) 0.170(19) Uiso 1 1 d G . . . .
H13 H 0.418190 0.400886 0.293684 0.204 Uiso 1 1 calc R . . . .
C14 C 0.3868(17) 0.3863(12) 0.3708(13) 0.29(4) Uiso 1 1 d G . . . .
H14 H 0.336374 0.409194 0.372465 0.350 Uiso 1 1 calc R . . . .
C15 C 0.4131(19) 0.3572(13) 0.4154(9) 0.158(17) Uiso 1 1 d G . . . .
H15 H 0.380310 0.360512 0.446987 0.190 Uiso 1 1 calc R . . . .
C16 C 0.488(2) 0.3230(11) 0.4129(8) 0.162(17) Uiso 1 1 d G . . . .
H16 H 0.506062 0.303521 0.442729 0.195 Uiso 1 1 calc R . . . .
C17 C 0.5375(14) 0.3181(8) 0.3657(10) 0.085(8) Uiso 1 1 d DG . . . .
N4 N 0.5476(9) 0.3914(5) 0.2047(5) 0.062(5) Uani 1 1 d . . . . .
C23 C 0.4876(11) 0.3685(5) 0.1679(7) 0.068(7) Uiso 1 1 d DG . . . .
C22 C 0.4497(12) 0.3995(8) 0.1274(6) 0.099(10) Uiso 1 1 d G . . . .
H22 H 0.409590 0.384195 0.102766 0.119 Uiso 1 1 calc R . . . .
C21 C 0.4717(13) 0.4533(7) 0.1238(6) 0.130(13) Uiso 1 1 d G . . . .
H21 H 0.446367 0.474030 0.096681 0.156 Uiso 1 1 calc R . . . .
C20 C 0.5317(13) 0.4762(5) 0.1606(7) 0.086(8) Uiso 1 1 d G . . . .
H20 H 0.546436 0.512193 0.158166 0.103 Uiso 1 1 calc R . . . .
C19 C 0.5696(10) 0.4452(5) 0.2011(6) 0.065(6) Uiso 1 1 d G . . . .
H19 H 0.609728 0.460520 0.225738 0.078 Uiso 1 1 calc R . . . .
N5 N 0.8669(10) 0.4221(6) 0.2965(5) 0.061(5) Uiso 1 1 d . . . . .
C29 C 0.8061(8) 0.4372(6) 0.3364(6) 0.064(6) Uiso 1 1 d DG . . . .
C28 C 0.8376(11) 0.4672(7) 0.3794(6) 0.102(10) Uiso 1 1 d G . . . .
H28 H 0.797003 0.477284 0.406122 0.122 Uiso 1 1 calc R . . . .
C27 C 0.9298(13) 0.4820(7) 0.3825(6) 0.116(11) Uiso 1 1 d G . . . .
H27 H 0.950917 0.502006 0.411246 0.139 Uiso 1 1 calc R . . . .
C26 C 0.9906(9) 0.4669(7) 0.3425(7) 0.075(7) Uiso 1 1 d G . . . .
H26 H 1.052262 0.476769 0.344591 0.090 Uiso 1 1 calc R . . . .
C25 C 0.9591(9) 0.4369(7) 0.2995(6) 0.087(9) Uiso 1 1 d G . . . .
H25 H 0.999694 0.426809 0.272813 0.105 Uiso 1 1 calc R . . . .
N6 N 0.7897(12) 0.4215(9) 0.1774(7) 0.068(6) Uani 1 1 d . . . . .
C35 C 0.7474(17) 0.3903(7) 0.1385(11) 0.116(11) Uiso 1 1 d DG . . . .
C34 C 0.7148(19) 0.4137(14) 0.0919(9) 0.240 Uiso 1 1 d G . . . .
H34 H 0.686480 0.392872 0.065890 0.287 Uiso 1 1 calc R . . . .
C33 C 0.724(2) 0.4683(15) 0.0841(9) 0.18(2) Uiso 1 1 d G . . . .
H33 H 0.702676 0.483998 0.052922 0.220 Uiso 1 1 calc R . . . .
C32 C 0.767(2) 0.4995(8) 0.1230(14) 0.26(3) Uiso 1 1 d G . . . .
H32 H 0.773271 0.536022 0.117765 0.309 Uiso 1 1 calc R . . . .
C31 C 0.7994(17) 0.4761(8) 0.1696(11) 0.18(2) Uiso 1 1 d G . . . .
H31 H 0.827671 0.496920 0.195575 0.212 Uiso 1 1 calc R . . . .
C6 C 0.532(2) 0.1567(17) 0.3012(14) 0.157(18) Uiso 1 1 d D . . . .
H6A H 0.574425 0.156730 0.331272 0.188 Uiso 1 1 calc R . . . .
H6B H 0.515749 0.119413 0.297022 0.188 Uiso 1 1 calc R . . . .
C12 C 0.6435(19) 0.1984(18) 0.1495(11) 0.145(15) Uiso 1 1 d D . . . .
H12A H 0.665806 0.230413 0.131977 0.175 Uiso 1 1 calc R . . . .
H12B H 0.680638 0.168630 0.137497 0.175 Uiso 1 1 calc R . . . .
C18 C 0.605(3) 0.2737(17) 0.3546(14) 0.18(2) Uiso 1 1 d D . . . .
H18A H 0.659200 0.277282 0.377185 0.214 Uiso 1 1 calc R . . . .
H18B H 0.576930 0.239264 0.361529 0.214 Uiso 1 1 calc R . . . .
C24 C 0.4773(15) 0.3101(7) 0.1729(8) 0.051(6) Uiso 1 1 d D . . . .
H24A H 0.412402 0.300959 0.171431 0.062 Uiso 1 1 calc R . . . .
H24B H 0.507604 0.292887 0.143114 0.062 Uiso 1 1 calc R . . . .
C30 C 0.7076(12) 0.4232(8) 0.3244(7) 0.044(5) Uiso 1 1 d D . . . .
H30A H 0.679355 0.408072 0.355982 0.053 Uiso 1 1 calc R . . . .
H30B H 0.673850 0.455187 0.314876 0.053 Uiso 1 1 calc R . . . .
C36 C 0.731(3) 0.3302(11) 0.1482(10) 0.119(12) Uiso 1 1 d D . . . .
H36A H 0.670853 0.320166 0.133716 0.143 Uiso 1 1 calc R . . . .
H36B H 0.777351 0.309526 0.129976 0.143 Uiso 1 1 calc R . . . .
Cl1 Cl 0.2412(5) 0.4211(4) 0.2483(4) 0.105(3) Uani 1 1 d D . . . .
O7 O 0.2536(12) 0.3650(8) 0.2487(7) 0.104(9) Uiso 1 1 d D . . . .
O10 O 0.312(2) 0.4511(17) 0.2256(17) 0.31(3) Uiso 1 1 d D . . . .
O8 O 0.1569(18) 0.4259(14) 0.2163(11) 0.202(14) Uiso 1 1 d D . . . .
O9 O 0.222(2) 0.4486(12) 0.2939(9) 0.179(13) Uiso 1 1 d D . . . .
N8 N 0.250000 0.437230 0.500000 0.060 Uiso 1 2 d DS T P . .
O14 O 0.250000 0.388190 0.500000 0.130 Uiso 1 2 d DS T P . .
O13 O 0.315450 0.465460 0.514110 0.141 Uiso 1 1 d D . . . .
N7 N 0.750000 0.355780 0.500000 0.106 Uiso 1 2 d DS T P . .
O12 O 0.732010 0.379160 0.457480 0.145 Uiso 1 1 d D . . . .
O11 O 0.750000 0.306220 0.500000 0.136 Uiso 1 2 d DS T 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
Cu1 O2 2.065(17) 7_655 ?
Cu1 O2 2.065(17) . ?
Cu1 O3 2.218(19) 7_655 ?
Cu1 O3 2.218(19) . ?
Cu1 O6 2.070(17) . ?
Cu1 O6 2.070(17) 7_655 ?
Cu2 O3 1.914(18) . ?
Cu2 O4 1.948(13) . ?
Cu2 O5 1.920(14) . ?
Cu2 O6 2.42(3) . ?
Cu2 N3 2.052(17) . ?
Cu2 N4 1.982(11) . ?
Cu3 O2 2.29(2) 7_655 ?
Cu3 O1 1.557(10) 7_655 ?
Cu3 O5 1.854(16) . ?
Cu3 O6 1.972(19) . ?
Cu3 N5 2.018(12) . ?
Cu3 N6 2.114(17) . ?
Cr1 O2 1.981(17) . ?
Cr1 O1 1.785(10) . ?
Cr1 O3 2.37(2) . ?
Cr1 O4 1.858(13) . ?
Cr1 N1 1.925(13) . ?
Cr1 N2 2.048(15) . ?
Cr1 C6 2.12(4) . ?
O2 C12 1.52(2) . ?
O1 C6 1.41(2) . ?
O3 C18 1.49(3) . ?
O4 C24 1.473(18) . ?
O5 C30 1.478(18) . ?
O6 C36 1.46(2) . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
C1 C2 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 C6 1.58(2) . ?
N2 C11 1.3900 . ?
N2 C7 1.3900 . ?
C11 C10 1.3900 . ?
C11 C12 1.51(2) . ?
C10 C9 1.3900 . ?
C9 C8 1.3900 . ?
C8 C7 1.3900 . ?
N3 C13 1.3900 . ?
N3 C17 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.51(3) . ?
N4 C23 1.3900 . ?
N4 C19 1.3900 . ?
C23 C22 1.3900 . ?
C23 C24 1.477(19) . ?
C22 C21 1.3900 . ?
C21 C20 1.3900 . ?
C20 C19 1.3900 . ?
N5 C29 1.3900 . ?
N5 C25 1.3900 . ?
C29 C28 1.3900 . ?
C29 C30 1.501(18) . ?
C28 C27 1.3900 . ?
C27 C26 1.3900 . ?
C26 C25 1.3900 . ?
N6 C35 1.3900 . ?
N6 C31 1.3900 . ?
C35 C34 1.3900 . ?
C35 C36 1.55(2) . ?
C34 C33 1.3900 . ?
C33 C32 1.3900 . ?
C32 C31 1.3900 . ?
Cl1 O7 1.42(2) . ?
Cl1 O10 1.40(2) . ?
Cl1 O8 1.47(2) . ?
Cl1 O9 1.37(2) . ?
N8 O14 1.2296 . ?
N8 O13 1.2347 . ?
N8 O13 1.2348 2_556 ?
N7 O12 1.2441 . ?
N7 O12 1.2440 2_656 ?
N7 O11 1.2426 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 180.0 7_655 . ?
O2 Cu1 O3 85.0(8) . . ?
O2 Cu1 O3 85.0(8) 7_655 7_655 ?
O2 Cu1 O3 95.0(8) 7_655 . ?
O2 Cu1 O3 95.0(8) . 7_655 ?
O2 Cu1 O6 83.5(8) 7_655 . ?
O2 Cu1 O6 83.5(8) . 7_655 ?
O2 Cu1 O6 96.5(8) 7_655 7_655 ?
O2 Cu1 O6 96.5(8) . . ?
O3 Cu1 O3 180.0 . 7_655 ?
O6 Cu1 O3 93.5(8) . 7_655 ?
O6 Cu1 O3 86.5(8) . . ?
O6 Cu1 O3 93.5(8) 7_655 . ?
O6 Cu1 O3 86.5(8) 7_655 7_655 ?
O6 Cu1 O6 180.0(5) . 7_655 ?
O3 Cu2 O4 80.6(8) . . ?
O3 Cu2 O5 97.6(8) . . ?
O3 Cu2 O6 84.5(7) . . ?
O3 Cu2 N3 78.9(9) . . ?
O3 Cu2 N4 163.9(9) . . ?
O4 Cu2 O6 95.4(6) . . ?
O4 Cu2 N3 90.5(7) . . ?
O4 Cu2 N4 83.4(6) . . ?
O5 Cu2 O4 166.3(6) . . ?
O5 Cu2 O6 70.9(6) . . ?
O5 Cu2 N3 102.5(7) . . ?
O5 Cu2 N4 97.4(6) . . ?
N3 Cu2 O6 161.2(8) . . ?
N4 Cu2 O6 94.9(6) . . ?
N4 Cu2 N3 103.5(8) . . ?
O1 Cu3 O2 54.5(6) 7_655 7_655 ?
O1 Cu3 O5 148.6(7) 7_655 . ?
O1 Cu3 O6 97.0(7) 7_655 . ?
O1 Cu3 N5 90.6(6) 7_655 . ?
O1 Cu3 N6 112.0(6) 7_655 . ?
O5 Cu3 O2 95.2(6) . 7_655 ?
O5 Cu3 O6 83.6(9) . . ?
O5 Cu3 N5 84.4(6) . . ?
O5 Cu3 N6 99.4(6) . . ?
O6 Cu3 O2 80.3(7) . 7_655 ?
O6 Cu3 N5 166.8(9) . . ?
O6 Cu3 N6 86.2(9) . . ?
N5 Cu3 O2 95.7(6) . 7_655 ?
N5 Cu3 N6 100.9(8) . . ?
N6 Cu3 O2 158.9(8) . 7_655 ?
O2 Cr1 O3 83.0(7) . . ?
O2 Cr1 N2 81.5(8) . . ?
O2 Cr1 C6 100.1(9) . . ?
O1 Cr1 O2 59.4(7) . . ?
O1 Cr1 O3 97.2(5) . . ?
O1 Cr1 O4 158.2(6) . . ?
O1 Cr1 N1 103.2(6) . . ?
O1 Cr1 N2 92.0(6) . . ?
O1 Cr1 C6 41.1(7) . . ?
O4 Cr1 O2 100.0(7) . . ?
O4 Cr1 O3 71.3(6) . . ?
O4 Cr1 N1 96.6(6) . . ?
O4 Cr1 N2 91.7(7) . . ?
O4 Cr1 C6 155.4(9) . . ?
N1 Cr1 O2 162.3(8) . . ?
N1 Cr1 O3 96.6(7) . . ?
N1 Cr1 N2 104.2(8) . . ?
N1 Cr1 C6 62.3(8) . . ?
N2 Cr1 O3 154.6(8) . . ?
N2 Cr1 C6 105.2(13) . . ?
C6 Cr1 O3 97.2(14) . . ?
Cu1 O2 Cu3 92.9(8) . 7_655 ?
Cr1 O2 Cu1 103.9(7) . . ?
Cr1 O2 Cu3 97.2(8) . 7_655 ?
C12 O2 Cu1 127.3(17) . . ?
C12 O2 Cu3 116(2) . 7_655 ?
C12 O2 Cr1 113.6(17) . . ?
Cu3 O1 Cr1 147.2(7) 7_655 . ?
C6 O1 Cu3 126.3(18) . 7_655 ?
C6 O1 Cr1 82.3(18) . . ?
Cu1 O3 Cr1 88.0(9) . . ?
Cu2 O3 Cu1 99.7(9) . . ?
Cu2 O3 Cr1 94.9(10) . . ?
C18 O3 Cu1 133.7(18) . . ?
C18 O3 Cu2 120.3(19) . . ?
C18 O3 Cr1 109(2) . . ?
Cr1 O4 Cu2 112.7(6) . . ?
C24 O4 Cu2 113.6(11) . . ?
C24 O4 Cr1 129.8(11) . . ?
Cu3 O5 Cu2 114.0(7) . . ?
C30 O5 Cu2 129.3(12) . . ?
C30 O5 Cu3 116.6(11) . . ?
Cu1 O6 Cu2 89.2(9) . . ?
Cu3 O6 Cu1 102.6(7) . . ?
Cu3 O6 Cu2 91.6(7) . . ?
C36 O6 Cu1 134.8(15) . . ?
C36 O6 Cu2 118.0(19) . . ?
C36 O6 Cu3 111.3(18) . . ?
C1 N1 Cr1 127.9(8) . . ?
C1 N1 C5 120.0 . . ?
C5 N1 Cr1 112.0(8) . . ?
N1 C1 C2 120.0 . . ?
C3 C2 C1 120.0 . . ?
C2 C3 C4 120.0 . . ?
C3 C4 C5 120.0 . . ?
N1 C5 C6 89.7(18) . . ?
C4 C5 N1 120.0 . . ?
C4 C5 C6 150.2(18) . . ?
C11 N2 Cr1 115.1(13) . . ?
C11 N2 C7 120.0 . . ?
C7 N2 Cr1 124.8(13) . . ?
N2 C11 C12 114.3(19) . . ?
C10 C11 N2 120.0 . . ?
C10 C11 C12 123(2) . . ?
C11 C10 C9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C9 C8 C7 120.0 . . ?
C8 C7 N2 120.0 . . ?
C13 N3 Cu2 125.3(15) . . ?
C13 N3 C17 120.0 . . ?
C17 N3 Cu2 114.4(15) . . ?
C14 C13 N3 120.0 . . ?
C15 C14 C13 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C17 120.0 . . ?
N3 C17 C18 115(2) . . ?
C16 C17 N3 120.0 . . ?
C16 C17 C18 124(2) . . ?
C23 N4 Cu2 114.8(9) . . ?
C23 N4 C19 120.0 . . ?
C19 N4 Cu2 125.1(9) . . ?
N4 C23 C24 114.6(13) . . ?
C22 C23 N4 120.0 . . ?
C22 C23 C24 125.1(13) . . ?
C23 C22 C21 120.0 . . ?
C22 C21 C20 120.0 . . ?
C19 C20 C21 120.0 . . ?
C20 C19 N4 120.0 . . ?
C29 N5 Cu3 112.9(9) . . ?
C29 N5 C25 120.0 . . ?
C25 N5 Cu3 126.5(9) . . ?
N5 C29 C30 113.4(12) . . ?
C28 C29 N5 120.0 . . ?
C28 C29 C30 126.3(12) . . ?
C27 C28 C29 120.0 . . ?
C28 C27 C26 120.0 . . ?
C25 C26 C27 120.0 . . ?
C26 C25 N5 120.0 . . ?
C35 N6 Cu3 105.9(16) . . ?
C35 N6 C31 120.0 . . ?
C31 N6 Cu3 133.5(16) . . ?
N6 C35 C34 120.0 . . ?
N6 C35 C36 121(2) . . ?
C34 C35 C36 119(2) . . ?
C33 C34 C35 120.0 . . ?
C34 C33 C32 120.0 . . ?
C33 C32 C31 120.0 . . ?
C32 C31 N6 120.0 . . ?
O1 C6 Cr1 56.6(14) . . ?
O1 C6 C5 152(3) . . ?
C5 C6 Cr1 96(2) . . ?
C11 C12 O2 111(2) . . ?
O3 C18 C17 107(3) . . ?
O4 C24 C23 111.6(16) . . ?
O5 C30 C29 110.8(15) . . ?
O6 C36 C35 110(2) . . ?
O7 Cl1 O8 101.1(16) . . ?
O10 Cl1 O7 116(2) . . ?
O10 Cl1 O8 110(2) . . ?
O9 Cl1 O7 121.4(17) . . ?
O9 Cl1 O10 103(3) . . ?
O9 Cl1 O8 103.9(19) . . ?
O14 N8 O13 125.0 . 2_556 ?
O14 N8 O13 125.0 . . ?
O13 N8 O13 110.0 . 2_556 ?
O12 N7 O12 123.8 2_656 . ?
O11 N7 O12 118.1 . 2_656 ?
O11 N7 O12 118.1 . . ?

_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 1.682
_oxdiff_exptl_absorpt_empirical_full_min 0.384
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               3
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 0.563(5) 8122 10908 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.126(3) 9459 9728 nmt -0.5005 -0.4997 -0.0004 1.4984 -0.4990 0.0052 0.0056
0.0033 0.9996
3 0.311(4) 8494 10597 nmt -0.4998 0.4998 -0.0016 -1.4978 -0.4997 -0.0024 0.0086
-0.0040 1.0009

_twin_special_details            
;
Component 2 rotated by 120.0851° 
 around [-0.00 0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct)
Component 3 rotated by -119.9041° 
 around [-0.00 0.00 1.00] (reciprocal) or [0.01 -0.00 1.00] (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_7
_database_code_depnum_ccdc_archive 'CCDC 1855226'
_audit_update_record             
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
# local name eb17001
_audit_creation_date             2017-11-07
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'1(C72 H84 Al6 Cu7 N12 O24), 6(Cl O4), 3(N0.67 O2), 21 (C H4 O)'
_chemical_formula_sum            'C93 H168 Al6 Cl6 Cu7 N14 O75'
_chemical_formula_weight         3501.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cu Al'
_chemical_oxdiff_usercomment     '@ 120 K 792o SE'
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'
Al Al 0.0645 0.0514 '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'
Cu Cu 0.3201 1.2651 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   27.8468(6)
_cell_length_b                   27.8468(6)
_cell_length_c                   17.6945(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11882.8(7)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    16493
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      27.1140
_cell_measurement_theta_min      3.7210
_shelx_estimated_absorpt_T_max   0.833
_shelx_estimated_absorpt_T_min   0.711
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0596 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.8957.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5421
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-29 0 -13 0.1037
-16 38 -5 0.1037
29 1 12 0.1271
16 -38 5 0.1133
-3 -32 -3 0.0924
-30 20 16 0.0919
-9 20 -21 0.0814
13 -23 20 0.0864
-3 -10 23 0.0691
35 -30 -7 0.1717
17 -4 -22 0.1289
-19 -1 -21 0.0914
13 -36 -9 0.1064
25 -13 19 0.1079
17 4 21 0.1100
-20 39 3 0.1060
-10 26 -18 0.0768
18 5 -19 0.1312
-8 7 24 0.0720
12 -11 -23 0.1152

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.165
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
-28.9967 0.0014 -13.0155 0.2174 0.8227 0.5248
-15.9988 37.9993 -5.0018 -0.1079 -0.4840 0.8591
28.9974 0.9977 12.0152 -0.1852 -0.8419 -0.4921
15.9988 -37.9993 5.0018 0.1079 0.4840 -0.8591
-2.9992 -31.9985 -3.0072 0.2081 0.8741 -0.4283
-30.0175 20.0241 16.0010 -0.9159 0.2105 0.3683
-8.9862 19.9846 -21.0099 0.6007 -0.1443 0.7661
12.9877 -22.9868 20.0103 -0.5181 0.1185 -0.8395
-3.0176 -9.9788 23.0085 -0.8162 0.2026 -0.5132
35.0118 -30.0179 -6.9966 0.6740 -0.1436 -0.7315
17.0195 -4.0251 -22.0057 0.9566 -0.2310 0.1250
-18.9888 -1.0094 -21.0163 0.5966 0.6282 0.5371
13.0084 -36.0098 -9.0055 0.5790 0.5861 -0.5608
24.9912 -12.9936 19.0152 -0.4173 -0.4327 -0.7903
16.9884 4.0100 21.0161 -0.6257 -0.6493 -0.4680
-20.0055 39.0075 3.0009 -0.4351 -0.4458 0.7833
-9.9884 25.9870 -18.0079 0.4602 -0.2802 0.8221
18.0177 4.9762 -19.0025 0.8217 -0.4921 0.2077
-8.0190 7.0227 24.0100 -0.9625 -0.0869 -0.2059
12.0190 -11.0232 -23.0088 0.9769 0.0751 0.0830

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49850
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.856
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  33.00   1.00   20.00    --   -7.39 -99.00-180.00   53
  2  ω    -45.00   3.00   1.00   20.00    --   -7.39  95.00 -16.00   48
  3  ω    -20.00  49.00   1.00   20.00    --    8.80 -99.00   0.00   69
  4  ω    -65.00  40.00   1.00   20.00    --    8.80 -77.00 120.00  105
  5  ω     -5.00  77.00   1.00   20.00    --    8.80  38.00 -30.00   82
  6  ω      2.00  32.00   1.00   20.00    --    8.80 -57.00   0.00   30
  7  ω    -59.00  39.00   1.00   20.00    --    8.80 -19.00 150.00   98
;
_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      0.0086807000
_diffrn_orient_matrix_UB_12      -0.0039297000
_diffrn_orient_matrix_UB_13      -0.0360400000
_diffrn_orient_matrix_UB_21      -0.0260452000
_diffrn_orient_matrix_UB_22      -0.0243869000
_diffrn_orient_matrix_UB_23      -0.0051867000
_diffrn_orient_matrix_UB_31      -0.0105685000
_diffrn_orient_matrix_UB_32      0.0159508000
_diffrn_orient_matrix_UB_33      -0.0167713000
_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_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4209
_reflns_number_total             4843
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 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         1.219
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4843
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0561
_refine_ls_restrained_S_all      1.063
_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)+(0.0895P)²+80.5735P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1697
_refine_special_details          
;
The SQUEEZE routine of PLATON accounted for electron density which corresponds with 21 molecules of methanol per complete wheel structure.  This diffuse electron density could not be modelled with discrete atoms.  The disordered nitrate counterion was modelled with fixed occupancies such that there are two nitrate per complete wheel (and six perchlorate) thus balancing the charges.

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
242_ALERT_2_B Low    'MainMol' Ueq as Compared to Neighbors of        Cl1 Check

Consequence of perchlorate disorder

420_ALERT_2_B D-H Without Acceptor       O3     --  H3     ...     Please Check
420_ALERT_2_B D-H Without Acceptor       O4     --  H4     ...     Please Check

Consequence of SQUEEZE

#===============================================================================
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.02 Report
202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent .........          1 Check

Isotropic nitrate, discussed above

220_ALERT_2_C Non-Solvent Resd 1   O   Ueq(max)/Ueq(min) Range        5.5 Ratio
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0085 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.707 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           7 Note
934_ALERT_3_C Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          1 Check
975_ALERT_2_C Check Calcd Residual Density  1.00A From    O104       0.73 eA-3
975_ALERT_2_C Check Calcd Residual Density  1.04A From    O103       0.56 eA-3
978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Note

There are no serious issues here.  This is a model for which a lot of solvent was handled with SQUEEZE.

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         15 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         11 Report

Noted

041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.2820 Check
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check

Missing solvent, masked by SQUEEZE, was included in total formula.

083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      80.57 Why ?
172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          2 Report
176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          2 Report
187_ALERT_4_G The CIF-Embedded .res File Contains RIGU Records          2 Report
300_ALERT_4_G Atom Site Occupancy of >O103   is Constrained at     0.6666 Check
300_ALERT_4_G Atom Site Occupancy of <O104   is Constrained at     0.3333 Check
300_ALERT_4_G Atom Site Occupancy of <N101   is Constrained at     0.3333 Check
301_ALERT_3_G Main Residue  Disorder ..............(Resd  1)..         12 % Note
302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  2)..        100 % Note
304_ALERT_4_G Non-Integer Number of Atoms (   2.67) in Resd. #          2 Check
432_ALERT_2_G Short Inter X...Y Contact  O6     ..  C2      ..       3.00 Ang.
606_ALERT_4_G VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.16 Ratio
860_ALERT_3_G Number of Least-Squares Restraints .............         88 Note
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note


There are no serious issues here.  This is a model for which a lot of solvent was handled with SQUEEZE.

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4 = O3-H3
 0.84 with sigma of 0.02
 O104-N101 = O103-N101
 1.25 with sigma of 0.02
 O6-O7 \\sim O6-O8 \\sim O8A-O6A \\sim O6A-O7A
 with sigma of 0.04
 Cl1-O5 \\sim Cl1-O6 \\sim Cl1-O7 \\sim Cl1-O8 \\sim Cl1-O8A \\sim Cl1-O6A
\\sim Cl1-O7A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl1, O5, O6, O6A, O7, O7A, O8, O8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O103, O104, N101
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O6A)=Sof(O7A)=Sof(O8A)=1-FVAR(1)
 Sof(O6)=Sof(O7)=Sof(O8)=FVAR(1)
 Fixed Sof: O103(0.6666) O104(0.33333) N101(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C4(H4A), C7(H7), C8(H8), C9(H9), C10(H10)
;
_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
Cu1 Cu 0.68185(2) 0.52394(2) 0.23077(3) 0.03388(19) Uani 1 1 d . . . . .
Cu2 Cu 0.666667 0.333333 0.333333 0.0242(3) Uani 1 6 d S T P . .
Al1 Al 0.61207(4) 0.40221(4) 0.33235(7) 0.0248(3) Uani 1 1 d . . . . .
O1 O 0.74008(11) 0.51203(11) 0.26993(17) 0.0339(7) Uani 1 1 d . . . . .
O2 O 0.61695(11) 0.45656(11) 0.26601(17) 0.0329(6) Uani 1 1 d . . . . .
O3 O 0.67198(10) 0.40042(10) 0.27853(15) 0.0261(6) Uani 1 1 d D . . . .
H3 H 0.6727(18) 0.4039(18) 0.2303(11) 0.031 Uiso 1 1 d DR . . . .
O4 O 0.55626(10) 0.34182(10) 0.27975(16) 0.0279(6) Uani 1 1 d D . . . .
H4 H 0.5544(19) 0.3423(19) 0.2325(11) 0.033 Uiso 1 1 d DR . . . .
N1 N 0.74101(15) 0.57405(15) 0.1595(2) 0.0398(9) Uani 1 1 d . . . . .
N2 N 0.62619(14) 0.54586(14) 0.2058(2) 0.0349(8) Uani 1 1 d . . . . .
C1 C 0.7343(2) 0.5946(2) 0.0951(3) 0.0583(14) Uani 1 1 d . . . . .
H1 H 0.698743 0.589529 0.083656 0.070 Uiso 1 1 calc R . . . .
C2 C 0.7770(3) 0.6231(3) 0.0442(4) 0.0725(18) Uani 1 1 d . . . . .
H2 H 0.771154 0.637495 -0.001414 0.087 Uiso 1 1 calc R . . . .
C3 C 0.8284(3) 0.6300(2) 0.0621(4) 0.0685(17) Uani 1 1 d . . . . .
H3A H 0.858743 0.649425 0.028489 0.082 Uiso 1 1 calc R . . . .
C4 C 0.8355(2) 0.6088(2) 0.1285(3) 0.0574(14) Uani 1 1 d . . . . .
H4A H 0.870687 0.613437 0.141435 0.069 Uiso 1 1 calc R . . . .
C5 C 0.79060(19) 0.58059(18) 0.1760(3) 0.0440(11) Uani 1 1 d . . . . .
C6 C 0.79404(18) 0.55641(18) 0.2502(3) 0.0460(12) Uani 1 1 d . . . . .
H6A H 0.820306 0.542343 0.246209 0.055 Uiso 1 1 calc R . . . .
H6B H 0.807690 0.585343 0.289901 0.055 Uiso 1 1 calc R . . . .
C7 C 0.6354(2) 0.59705(19) 0.1899(3) 0.0424(10) Uani 1 1 d . . . . .
H7 H 0.672402 0.627283 0.190077 0.051 Uiso 1 1 calc R . . . .
C8 C 0.5927(2) 0.6068(2) 0.1732(3) 0.0478(12) Uani 1 1 d . . . . .
H8 H 0.600090 0.643213 0.161653 0.057 Uiso 1 1 calc R . . . .
C9 C 0.5394(2) 0.5631(2) 0.1736(3) 0.0469(12) Uani 1 1 d . . . . .
H9 H 0.509502 0.568940 0.161145 0.056 Uiso 1 1 calc R . . . .
C10 C 0.52910(19) 0.5108(2) 0.1922(2) 0.0397(10) Uani 1 1 d . . . . .
H10 H 0.492297 0.480269 0.193835 0.048 Uiso 1 1 calc R . . . .
C11 C 0.57453(18) 0.50386(17) 0.2085(2) 0.0339(9) Uani 1 1 d . . . . .
C12 C 0.56808(18) 0.44857(18) 0.2291(3) 0.0418(10) Uani 1 1 d . . . . .
H12A H 0.535739 0.428374 0.262959 0.050 Uiso 1 1 calc R . . . .
H12B H 0.561499 0.426054 0.182879 0.050 Uiso 1 1 calc R . . . .
Cl1 Cl 0.69455(5) 0.62993(5) 0.38585(8) 0.0538(3) Uani 1 1 d D U . . .
O5 O 0.71101(15) 0.59917(15) 0.3381(2) 0.0553(9) Uani 1 1 d D U . . .
O6 O 0.6362(3) 0.6039(5) 0.3820(7) 0.076(4) Uani 0.483(15) 1 d D U . A 1
O6A O 0.6566(6) 0.6436(8) 0.3576(7) 0.114(7) Uani 0.517(15) 1 d D U . A 2
O7 O 0.7158(9) 0.6398(11) 0.4565(7) 0.145(10) Uani 0.483(15) 1 d D U . A 1
O7A O 0.6747(9) 0.5990(5) 0.4548(7) 0.144(7) Uani 0.517(15) 1 d D U . A 2
O8 O 0.7146(6) 0.6802(4) 0.3448(9) 0.115(7) Uani 0.483(15) 1 d D U . A 1
O8A O 0.7428(3) 0.6785(4) 0.4147(8) 0.084(5) Uani 0.517(15) 1 d D U . A 2
O103 O 0.5134(7) 0.4661(7) 0.0101(9) 0.201(6) Uiso 0.6666 1 d D U . . .
O104 O 0.5833(9) 0.5517(9) -0.0249(13) 0.139(7) Uiso 0.3333 1 d D U . . .
N101 N 0.5321(8) 0.5149(8) -0.0082(11) 0.094(6) Uiso 0.3333 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.938(3) . ?
Cu1 O2 1.945(3) . ?
Cu1 N1 1.988(4) . ?
Cu1 N2 1.979(3) . ?
Cu2 Al1 2.9848(10) 16_655 ?
Cu2 Al1 2.9844(11) 17 ?
Cu2 Al1 2.9845(11) . ?
Cu2 Al1 2.9845(10) 3_665 ?
Cu2 Al1 2.9844(11) 18_545 ?
Cu2 Al1 2.9845(11) 2_655 ?
Cu2 O3 2.043(3) 3_665 ?
Cu2 O3 2.043(3) . ?
Cu2 O3 2.043(3) 17 ?
Cu2 O3 2.043(3) 2_655 ?
Cu2 O3 2.043(3) 16_655 ?
Cu2 O3 2.043(3) 18_545 ?
Al1 Al1 2.9848(10) 17 ?
Al1 Al1 2.9848(11) 18_545 ?
Al1 O1 1.866(3) 18_545 ?
Al1 O2 1.866(3) . ?
Al1 O3 1.943(3) . ?
Al1 O3 1.948(3) 18_545 ?
Al1 O4 1.874(3) 17 ?
Al1 O4 1.870(3) . ?
O1 C6 1.432(5) . ?
O2 C12 1.423(5) . ?
O3 H3 0.859(19) . ?
O4 H4 0.838(19) . ?
N1 C1 1.330(7) . ?
N1 C5 1.332(6) . ?
N2 C7 1.346(5) . ?
N2 C11 1.326(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.381(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.383(10) . ?
C3 H3A 0.9500 . ?
C3 C4 1.373(9) . ?
C4 H4A 0.9500 . ?
C4 C5 1.381(7) . ?
C5 C6 1.501(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.378(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.371(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.377(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.402(6) . ?
C11 C12 1.503(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Cl1 O5 1.432(3) . ?
Cl1 O6 1.411(8) . ?
Cl1 O6A 1.385(8) . ?
Cl1 O7 1.352(9) . ?
Cl1 O7A 1.434(9) . ?
Cl1 O8 1.421(9) . ?
Cl1 O8A 1.441(8) . ?
O103 N101 1.231(15) . ?
O103 N101 1.60(2) 10_665 ?
O104 N101 1.308(17) . ?
N101 N101 1.57(4) 10_665 ?

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 Cu1 O2 100.00(11) . . ?
O1 Cu1 N1 82.89(14) . . ?
O1 Cu1 N2 169.68(14) . . ?
O2 Cu1 N1 157.59(15) . . ?
O2 Cu1 N2 82.87(13) . . ?
N2 Cu1 N1 98.27(15) . . ?
Al1 Cu2 Al1 180.0 16_655 . ?
Al1 Cu2 Al1 60.002(1) 2_655 16_655 ?
Al1 Cu2 Al1 180.0 2_655 17 ?
Al1 Cu2 Al1 119.995(1) 3_665 . ?
Al1 Cu2 Al1 119.997(1) 3_665 2_655 ?
Al1 Cu2 Al1 119.993(1) 18_545 16_655 ?
Al1 Cu2 Al1 59.997(1) 3_665 17 ?
Al1 Cu2 Al1 119.998(1) 2_655 . ?
Al1 Cu2 Al1 60.007(1) 18_545 . ?
Al1 Cu2 Al1 60.005(1) 3_665 16_655 ?
Al1 Cu2 Al1 119.992(1) 17 16_655 ?
Al1 Cu2 Al1 180.0 3_665 18_545 ?
Al1 Cu2 Al1 120.005(1) 18_545 17 ?
Al1 Cu2 Al1 60.008(1) 17 . ?
Al1 Cu2 Al1 60.001(1) 2_655 18_545 ?
O3 Cu2 Al1 89.60(7) 16_655 18_545 ?
O3 Cu2 Al1 139.72(7) . 16_655 ?
O3 Cu2 Al1 139.73(7) 2_655 17 ?
O3 Cu2 Al1 40.27(7) 16_655 16_655 ?
O3 Cu2 Al1 139.72(7) 18_545 3_665 ?
O3 Cu2 Al1 40.39(7) 3_665 16_655 ?
O3 Cu2 Al1 40.39(7) 17 3_665 ?
O3 Cu2 Al1 40.27(7) 3_665 3_665 ?
O3 Cu2 Al1 89.60(7) . 3_665 ?
O3 Cu2 Al1 90.39(7) 18_545 2_655 ?
O3 Cu2 Al1 40.28(7) 18_545 18_545 ?
O3 Cu2 Al1 139.61(7) 2_655 3_665 ?
O3 Cu2 Al1 40.27(7) . . ?
O3 Cu2 Al1 40.39(7) 2_655 18_545 ?
O3 Cu2 Al1 40.40(7) 18_545 . ?
O3 Cu2 Al1 139.61(7) 17 18_545 ?
O3 Cu2 Al1 139.60(7) 18_545 16_655 ?
O3 Cu2 Al1 40.40(7) . 17 ?
O3 Cu2 Al1 90.39(7) 2_655 16_655 ?
O3 Cu2 Al1 139.60(7) . 2_655 ?
O3 Cu2 Al1 90.39(7) 3_665 17 ?
O3 Cu2 Al1 89.61(7) 18_545 17 ?
O3 Cu2 Al1 139.72(7) 3_665 18_545 ?
O3 Cu2 Al1 89.60(7) 17 16_655 ?
O3 Cu2 Al1 40.27(7) 17 17 ?
O3 Cu2 Al1 40.27(7) 2_655 2_655 ?
O3 Cu2 Al1 89.60(7) 3_665 2_655 ?
O3 Cu2 Al1 40.40(7) 16_655 2_655 ?
O3 Cu2 Al1 89.60(7) 2_655 . ?
O3 Cu2 Al1 90.40(7) . 18_545 ?
O3 Cu2 Al1 90.39(7) 16_655 3_665 ?
O3 Cu2 Al1 90.40(7) 17 . ?
O3 Cu2 Al1 139.72(7) 17 2_655 ?
O3 Cu2 Al1 139.60(7) 3_665 . ?
O3 Cu2 Al1 139.60(7) 16_655 17 ?
O3 Cu2 Al1 139.73(7) 16_655 . ?
O3 Cu2 O3 180.0 2_655 17 ?
O3 Cu2 O3 80.67(9) 17 . ?
O3 Cu2 O3 99.33(9) 2_655 . ?
O3 Cu2 O3 80.67(9) . 18_545 ?
O3 Cu2 O3 80.66(9) 3_665 16_655 ?
O3 Cu2 O3 80.67(9) 2_655 18_545 ?
O3 Cu2 O3 99.33(9) 16_655 18_545 ?
O3 Cu2 O3 180.0 16_655 . ?
O3 Cu2 O3 99.34(9) 17 18_545 ?
O3 Cu2 O3 99.33(9) 3_665 . ?
O3 Cu2 O3 80.66(9) 3_665 17 ?
O3 Cu2 O3 180.0 3_665 18_545 ?
O3 Cu2 O3 99.34(9) 3_665 2_655 ?
O3 Cu2 O3 99.33(9) 16_655 17 ?
O3 Cu2 O3 80.67(9) 2_655 16_655 ?
Cu2 Al1 Al1 59.995(1) . 17 ?
Cu2 Al1 Al1 60.0 . 18_545 ?
Al1 Al1 Al1 119.979(2) 18_545 17 ?
O1 Al1 Cu2 133.26(10) 18_545 . ?
O1 Al1 Al1 132.53(11) 18_545 17 ?
O1 Al1 Al1 89.93(9) 18_545 18_545 ?
O1 Al1 O3 90.85(13) 18_545 18_545 ?
O1 Al1 O3 171.41(14) 18_545 . ?
O1 Al1 O4 95.44(13) 18_545 17 ?
O1 Al1 O4 92.76(13) 18_545 . ?
O2 Al1 Cu2 132.15(10) . . ?
O2 Al1 Al1 133.32(11) . 18_545 ?
O2 Al1 Al1 89.77(9) . 17 ?
O2 Al1 O1 94.59(13) . 18_545 ?
O2 Al1 O3 89.84(13) . . ?
O2 Al1 O3 171.40(14) . 18_545 ?
O2 Al1 O4 96.15(13) . . ?
O2 Al1 O4 93.46(13) . 17 ?
O3 Al1 Cu2 42.82(8) . . ?
O3 Al1 Cu2 42.83(8) 18_545 . ?
O3 Al1 Al1 39.86(8) 18_545 18_545 ?
O3 Al1 Al1 92.38(8) . 18_545 ?
O3 Al1 Al1 39.96(8) . 17 ?
O3 Al1 Al1 91.46(8) 18_545 17 ?
O3 Al1 O3 85.65(16) . 18_545 ?
O4 Al1 Cu2 83.47(8) . . ?
O4 Al1 Cu2 83.40(8) 17 . ?
O4 Al1 Al1 37.08(9) 17 17 ?
O4 Al1 Al1 132.36(10) 17 18_545 ?
O4 Al1 Al1 133.76(10) . 17 ?
O4 Al1 Al1 37.18(9) . 18_545 ?
O4 Al1 O3 92.65(12) 17 18_545 ?
O4 Al1 O3 76.92(12) 17 . ?
O4 Al1 O3 94.08(12) . . ?
O4 Al1 O3 76.91(12) . 18_545 ?
O4 Al1 O4 166.82(15) . 17 ?
Al1 O1 Cu1 129.89(14) 17 . ?
C6 O1 Cu1 111.8(2) . . ?
C6 O1 Al1 118.0(3) . 17 ?
Al1 O2 Cu1 129.77(14) . . ?
C12 O2 Cu1 111.0(2) . . ?
C12 O2 Al1 119.1(2) . . ?
Cu2 O3 H3 124(3) . . ?
Al1 O3 Cu2 96.76(12) 17 . ?
Al1 O3 Cu2 96.91(12) . . ?
Al1 O3 Al1 100.18(12) . 17 ?
Al1 O3 H3 117(3) 17 . ?
Al1 O3 H3 117(3) . . ?
Al1 O4 Al1 105.74(14) . 18_545 ?
Al1 O4 H4 123(3) 18_545 . ?
Al1 O4 H4 121(3) . . ?
C1 N1 Cu1 126.9(4) . . ?
C1 N1 C5 119.2(4) . . ?
C5 N1 Cu1 113.3(3) . . ?
C7 N2 Cu1 127.5(3) . . ?
C11 N2 Cu1 113.1(3) . . ?
C11 N2 C7 119.4(4) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.8(6) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 121.2 . . ?
C1 C2 C3 117.6(6) . . ?
C3 C2 H2 121.2 . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 C2 119.9(5) . . ?
C4 C3 H3A 120.1 . . ?
C3 C4 H4A 120.6 . . ?
C3 C4 C5 118.8(5) . . ?
C5 C4 H4A 120.6 . . ?
N1 C5 C4 121.8(5) . . ?
N1 C5 C6 115.1(4) . . ?
C4 C5 C6 123.1(5) . . ?
O1 C6 C5 109.0(4) . . ?
O1 C6 H6A 109.9 . . ?
O1 C6 H6B 109.9 . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N2 C7 H7 119.1 . . ?
N2 C7 C8 121.8(5) . . ?
C8 C7 H7 119.1 . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.8(4) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.1(4) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 121.0 . . ?
C9 C10 C11 118.0(4) . . ?
C11 C10 H10 121.0 . . ?
N2 C11 C10 121.8(4) . . ?
N2 C11 C12 115.7(4) . . ?
C10 C11 C12 122.5(4) . . ?
O2 C12 C11 109.6(3) . . ?
O2 C12 H12A 109.7 . . ?
O2 C12 H12B 109.7 . . ?
C11 C12 H12A 109.7 . . ?
C11 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O5 Cl1 O7A 106.6(7) . . ?
O5 Cl1 O8A 110.1(4) . . ?
O6 Cl1 O5 107.2(5) . . ?
O6 Cl1 O8 105.5(8) . . ?
O6A Cl1 O5 118.0(5) . . ?
O6A Cl1 O7A 110.7(10) . . ?
O6A Cl1 O8A 110.6(8) . . ?
O7 Cl1 O5 115.4(6) . . ?
O7 Cl1 O6 115.0(10) . . ?
O7 Cl1 O8 110.9(13) . . ?
O7A Cl1 O8A 99.2(8) . . ?
O8 Cl1 O5 101.7(5) . . ?
N101 O103 N101 66.2(18) . 10_665 ?
O103 N101 O103 113.8(18) . 10_665 ?
O103 N101 O104 128(2) . . ?
O103 N101 N101 68.2(15) . 10_665 ?
O104 N101 O103 118(2) . 10_665 ?
O104 N101 N101 164(3) . 10_665 ?
N101 N101 O103 45.7(10) 10_665 10_665 ?

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
Cu1 O1 C6 C5 -30.4(4) . . . . ?
Cu1 O2 C12 C11 -29.7(4) . . . . ?
Cu1 N1 C1 C2 -171.1(5) . . . . ?
Cu1 N1 C5 C4 172.7(4) . . . . ?
Cu1 N1 C5 C6 -8.7(5) . . . . ?
Cu1 N2 C7 C8 180.0(4) . . . . ?
Cu1 N2 C11 C10 -179.6(3) . . . . ?
Cu1 N2 C11 C12 -0.3(5) . . . . ?
Cu2 Al1 O2 Cu1 -54.1(3) . . . . ?
Cu2 Al1 O2 C12 120.7(3) . . . . ?
Cu2 Al1 O4 Al1 47.00(10) . . . 18_545 ?
Al1 Al1 O2 Cu1 -6.8(2) 17 . . . ?
Al1 Al1 O2 Cu1 -139.92(15) 18_545 . . . ?
Al1 Al1 O2 C12 34.9(4) 18_545 . . . ?
Al1 Al1 O2 C12 168.0(3) 17 . . . ?
Al1 Al1 O4 Al1 83.24(16) 17 . . 18_545 ?
Al1 O1 C6 C5 155.2(3) 17 . . . ?
Al1 O2 C12 C11 154.5(3) . . . . ?
O1 Al1 O2 Cu1 125.8(2) 18_545 . . . ?
O1 Al1 O2 C12 -59.3(3) 18_545 . . . ?
O1 Al1 O4 Al1 -86.24(16) 18_545 . . 18_545 ?
O2 Al1 O4 Al1 178.84(14) . . . 18_545 ?
O3 Al1 O2 Cu1 -46.8(2) . . . . ?
O3 Al1 O2 C12 128.0(3) . . . . ?
O3 Al1 O4 Al1 3.99(13) 18_545 . . 18_545 ?
O3 Al1 O4 Al1 88.56(13) . . . 18_545 ?
O4 Al1 O2 Cu1 -140.9(2) . . . . ?
O4 Al1 O2 Cu1 30.1(2) 17 . . . ?
O4 Al1 O2 C12 -155.1(3) 17 . . . ?
O4 Al1 O2 C12 33.9(3) . . . . ?
O4 Al1 O4 Al1 42.3(4) 17 . . 18_545 ?
N1 C1 C2 C3 0.1(10) . . . . ?
N1 C5 C6 O1 25.6(6) . . . . ?
N2 C7 C8 C9 0.6(7) . . . . ?
N2 C11 C12 O2 19.8(6) . . . . ?
C1 N1 C5 C4 0.8(7) . . . . ?
C1 N1 C5 C6 179.4(5) . . . . ?
C1 C2 C3 C4 0.0(10) . . . . ?
C2 C3 C4 C5 0.3(9) . . . . ?
C3 C4 C5 N1 -0.7(8) . . . . ?
C3 C4 C5 C6 -179.2(5) . . . . ?
C4 C5 C6 O1 -155.8(4) . . . . ?
C5 N1 C1 C2 -0.5(8) . . . . ?
C7 N2 C11 C10 2.6(6) . . . . ?
C7 N2 C11 C12 -178.1(4) . . . . ?
C7 C8 C9 C10 1.5(7) . . . . ?
C8 C9 C10 C11 -1.5(7) . . . . ?
C9 C10 C11 N2 -0.6(7) . . . . ?
C9 C10 C11 C12 -179.8(4) . . . . ?
C10 C11 C12 O2 -160.9(4) . . . . ?
C11 N2 C7 C8 -2.6(7) . . . . ?
N101 O103 N101 O103 0.000(1) 10_665 . . 10_665 ?
N101 O103 N101 O104 179(3) 10_665 . . . ?

_olex2_date_sample_data_collection 2017-01-11
_olex2_date_sample_submission    2017-01-11
_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 '792o SE'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.211
_oxdiff_exptl_absorpt_empirical_full_min 0.865
_vrf_CHEMW03_7                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Consequence of SQUEEZE.  Please see the _refine_special_details section of the CIF.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1855227'
_audit_update_record             
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
# local name eb16271
_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         'C72 H72 Cr2 Fe5 N12 O12, 4(Cl1 O4), 9 C H4 O'
_chemical_formula_sum            'C81 H108 Cl4 Cr2 Fe5 N12 O37'
_chemical_formula_weight         2366.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr2 Fe5 Cl2'
_chemical_oxdiff_usercomment     '@ 120 K 788o '
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'
Fe Fe -1.1336 3.1974 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   14.6087(3)
_cell_length_b                   14.6087(3)
_cell_length_c                   37.9381(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7011.8(5)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    7747
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      73.0590
_cell_measurement_theta_min      4.1670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.765
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.731
_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 brown'
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3660
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 -5 -4 0.0396
8 -8 4 0.0740
-8 8 -4 0.0531
-1 8 1 0.0457
8 1 6 0.0502
0 0 1 0.0167
0 0 -1 0.0167

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.033
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-4.0018 -5.0020 -3.9978 0.0428 -0.1345 0.9547
7.9955 -8.0021 4.0015 -0.2727 0.9323 0.1785
-7.9955 8.0021 -4.0015 0.2727 -0.9323 -0.1785
-0.9962 8.0026 0.9975 0.1091 -0.3743 -0.8340
7.9996 1.0010 5.9985 -0.1791 0.6006 -0.8655
0.0001 0.0001 0.9998 -0.0401 -0.0036 -0.0056
-0.0001 -0.0001 -0.9998 0.0401 0.0036 0.0056

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            32839
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.728
_diffrn_reflns_theta_min         3.495
_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 1.0000
_diffrn_measured_fraction_theta_max 0.9900
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  -2.00   1.00   15.00    --  -43.17 125.00  30.00   94
  2  ω    -96.00  -2.00   1.00   15.00    --  -43.17 125.00 120.00   94
  3  ω   -116.00 -21.00   1.00   15.00    --  -43.17 -38.00  30.00   95
  4  ω   -116.00 -21.00   1.00   15.00    --  -43.17 -38.00 -60.00   95
  5  ω      1.00  83.00   1.00   15.00    --   43.17 -99.00 -90.00   82
  6  ω     30.00 109.00   1.00   25.00    --  111.00 -94.00-120.00   79
  7  ω     87.00 178.00   1.00   25.00    --  111.00  45.00 -60.00   91
  8  ω     41.00 139.00   1.00   25.00    --  111.00 -61.00   0.00   98
  9  ω     38.00 118.00   1.00   25.00    --  111.00-118.00 141.00   80
 10  ω     37.00 142.00   1.00   25.00    --  111.00 -77.00-120.00  105
 11  ω     36.00 135.00   1.00   25.00    --  111.00 -30.00 -30.00   99
 12  ω     39.00 121.00   1.00   25.00    --  111.00-125.00  30.00   82
 13  ω     87.00 178.00   1.00   25.00    --  111.00  45.00 -30.00   91
 14  ω     40.00 135.00   1.00   25.00    --  111.00 -45.00  90.00   95
 15  ω     41.00 139.00   1.00   25.00    --  111.00 -61.00-150.00   98
 16  ω     30.00 109.00   1.00   25.00    --  111.00 -94.00   0.00   79
 17  ω     87.00 178.00   1.00   25.00    --  111.00  30.00 -90.00   91
 18  ω     30.00 109.00   1.00   25.00    --  111.00 -94.00  30.00   79
 19  ω     39.00 121.00   1.00   25.00    --  111.00-125.00-150.00   82
 20  ω     87.00 178.00   1.00   25.00    --  111.00  45.00   0.00   91
 21  ω     39.00 121.00   1.00   25.00    --  111.00-125.00 120.00   82
 22  ω     84.00 116.00   1.00   25.00    --  111.00-125.00   0.00   32
 23  ω     45.00 120.00   1.00   25.00    --  111.00-125.00-180.00   75
 24  ω     47.00 121.00   1.00   25.00    --  111.00-125.00-120.00   74
 25  ω    108.00 171.00   1.00   25.00    --  111.00  15.00  60.00   63
;
_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      0.0052394000
_diffrn_orient_matrix_UB_12      0.0192787000
_diffrn_orient_matrix_UB_13      -0.0400609000
_diffrn_orient_matrix_UB_21      0.0822667000
_diffrn_orient_matrix_UB_22      -0.0360845000
_diffrn_orient_matrix_UB_23      -0.0035575000
_diffrn_orient_matrix_UB_31      -0.0896489000
_diffrn_orient_matrix_UB_32      -0.1146778000
_diffrn_orient_matrix_UB_33      -0.0055940000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\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                2673
_reflns_number_total             3272
_reflns_odcompleteness_completeness 100.00
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 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         1.455
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3272
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0712
_refine_ls_restrained_S_all      1.068
_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)+(0.1458P)²+13.1062P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2052
_refine_ls_wR_factor_ref         0.2197
_refine_special_details          
;
The occupancies of the metal sites were constrained such that the total number of metals per complete wheel are Cr2Fe5.  This is consistent with charge balance and other analytical data.  Nine molecule of MeOH per asymmetric unit were handled using the SQUEEZE routine of PLATON.  This missing solvent was included in the total formula, triggering checkCIF alerts which should be ignored. One of the perchlorate anions was modelled as disordered over two sites.  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
 
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        Cl1 Check
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0095 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.083 Check
934_ALERT_3_C Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          1 Check

All checked and not significant

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          8 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          8 Report

Noted

041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.2053 Check
051_ALERT_1_G Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       1.56 %
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.15 Report
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      13.11 Why ?
171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records          1 Report
176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          5 Report
187_ALERT_4_G The CIF-Embedded .res File Contains RIGU Records          2 Report

ALl a consequence of SQUEEZE and disorder

232_ALERT_2_G Hirshfeld Test Diff (M-X)  Fe1    --  O1      ..        5.4 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Fe1    --  O2      ..        5.0 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Fe1    --  N1      ..        5.5 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  O1      ..        5.4 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  O2      ..        5.0 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  N1      ..        5.5 s.u.
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
300_ALERT_4_G Atom Site Occupancy of >Fe1    is Constrained at     0.6667 Check
300_ALERT_4_G Atom Site Occupancy of <Cr1    is Constrained at     0.3333 Check
301_ALERT_3_G Main Residue  Disorder ............ Percentage =          4 Note
302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =         40 Note
605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        474 A**3
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        113 Check
              O3   -CL1  -O3A     2.655   1.555   2.655             27.20 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        115 Check
              O3   -CL1  -O3A     3.665   1.555   3.665             27.20 Deg.
860_ALERT_3_G Number of Least-Squares Restraints .............         37 Note
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         32 Note

Noted, but not important.

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Fe1, Cr1}
3. Restrained distances
 O4-O3 \\sim O5-O6
 with sigma of 0.02
 Cl1-O3 \\sim Cl1-O4 \\sim Cl1-O3A
 with sigma of 0.02
 Cl1-O3 \\sim Cl1-O4 \\sim Cl1-O3A \\sim Cl1-O4A
 with sigma of 0.02
 O4A-O3A \\sim O3-O4
 with sigma of 0.02
 Cl2-O5 \\sim Cl2-O6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Cr1)
5. Rigid body (RIGU) restrains
 Cl2, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O3A, O4, O3, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O3A)=1-FVAR(1)
 Sof(O4A)=0.3333*(1-FVAR(2))
 Sof(O4)=0.33333*FVAR(2)
 Sof(O3)=FVAR(1)
 Fixed Sof: Fe1(0.66667) Cr1(0.3333)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     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
Fe1 Fe 0.57523(5) 0.72878(5) 0.17034(2) 0.0421(3) Uani 0.6667 1 d . . . A 1
Fe2 Fe 0.333333 0.666667 0.166667 0.0375(3) Uani 1 6 d S T P A .
Cr1 Cr 0.57523(5) 0.72878(5) 0.17034(2) 0.0421(3) Uani 0.3333 1 d . . . A 2
O1 O 0.4742(2) 0.7703(2) 0.19441(9) 0.0462(7) Uani 1 1 d . . . . .
O2 O 0.5248(2) 0.5854(2) 0.18936(9) 0.0472(7) Uani 1 1 d . . . . .
N1 N 0.6617(3) 0.8044(3) 0.21514(12) 0.0534(9) Uani 1 1 d . . . . .
N2 N 0.4057(3) 0.3830(3) 0.19806(11) 0.0494(8) Uani 1 1 d . . . . .
C1 C 0.7622(4) 0.8368(4) 0.22166(17) 0.0653(13) Uani 1 1 d . . . . .
H1 H 0.802946 0.828651 0.203718 0.078 Uiso 1 1 calc R . . . .
C2 C 0.8107(5) 0.8816(5) 0.2529(2) 0.0820(19) Uani 1 1 d . . . . .
H2 H 0.883338 0.904141 0.256409 0.098 Uiso 1 1 calc R . . . .
C3 C 0.7520(5) 0.8935(6) 0.2796(2) 0.0873(19) Uani 1 1 d . . . . .
H3 H 0.783132 0.922052 0.301846 0.105 Uiso 1 1 calc R . . . .
C4 C 0.6476(5) 0.8629(5) 0.27304(16) 0.0736(15) Uani 1 1 d . . . . .
H4 H 0.606336 0.871944 0.290546 0.088 Uiso 1 1 calc R . . . .
C5 C 0.6037(4) 0.8190(4) 0.24083(13) 0.0555(11) Uani 1 1 d . . . . .
C6 C 0.4891(4) 0.7815(4) 0.23177(13) 0.0539(11) Uani 1 1 d . . . . .
H6A H 0.442784 0.712795 0.243362 0.065 Uiso 1 1 calc R . . . .
H6B H 0.469456 0.833193 0.240581 0.065 Uiso 1 1 calc R . . . .
C7 C 0.3367(4) 0.2789(3) 0.20151(16) 0.0609(13) Uani 1 1 d . . . . .
H7 H 0.279162 0.246124 0.185476 0.073 Uiso 1 1 calc R . . . .
C8 C 0.3461(5) 0.2183(4) 0.22726(19) 0.0775(18) Uani 1 1 d . . . . .
H8 H 0.295369 0.145281 0.229158 0.093 Uiso 1 1 calc R . . . .
C9 C 0.4299(6) 0.2645(5) 0.2503(2) 0.0840(19) Uani 1 1 d . . . . .
H9 H 0.437694 0.223600 0.268291 0.101 Uiso 1 1 calc R . . . .
C10 C 0.5021(5) 0.3703(5) 0.24711(18) 0.0741(15) Uani 1 1 d . . . . .
H10 H 0.561363 0.403444 0.262440 0.089 Uiso 1 1 calc R . . . .
C11 C 0.4866(4) 0.4281(4) 0.22084(14) 0.0544(11) Uani 1 1 d . . . . .
C12 C 0.5619(4) 0.5447(4) 0.21584(14) 0.0569(12) Uani 1 1 d . . . . .
H12A H 0.569193 0.582373 0.238267 0.068 Uiso 1 1 calc R . . . .
H12B H 0.632496 0.556254 0.209204 0.068 Uiso 1 1 calc R . . . .
Cl1 Cl 0.666667 0.333333 0.17044(8) 0.0728(6) Uani 1 3 d DS TU P . .
O3 O 0.6965(11) 0.4365(6) 0.1620(3) 0.077(3) Uani 0.70(2) 1 d D U . B 1
O3A O 0.694(3) 0.4375(15) 0.1793(7) 0.105(10) Uani 0.30(2) 1 d D U . B 2
O4 O 0.666667 0.333333 0.2100(3) 0.128(6) Uani 0.70(2) 3 d DS TU P B 1
O4A O 0.666667 0.333333 0.1317(4) 0.20(2) Uani 0.30(2) 3 d DS TU P B 2
Cl2 Cl 1.000000 1.000000 0.34507(7) 0.0868(8) Uani 1 3 d DS TU P . .
O5 O 1.000000 1.000000 0.30806(19) 0.095(2) Uani 1 3 d DS TU P C .
O6 O 0.9200(8) 1.0194(10) 0.3584(2) 0.203(5) Uani 1 1 d D U . C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.068(3) . ?
Fe1 O1 2.162(3) 14_455 ?
Fe1 O2 1.976(3) . ?
Fe1 O2 1.981(3) 15 ?
Fe1 N1 2.076(4) . ?
Fe1 N2 2.079(4) 15 ?
Fe2 O1 2.126(3) 2_665 ?
Fe2 O1 2.126(3) 3_565 ?
Fe2 O1 2.126(3) 13_565 ?
Fe2 O1 2.126(3) . ?
Fe2 O1 2.126(3) 14_455 ?
Fe2 O1 2.126(3) 15 ?
Cr1 O1 2.162(3) 14_455 ?
Cr1 O1 2.068(3) . ?
Cr1 O2 1.976(3) . ?
Cr1 O2 1.981(3) 15 ?
Cr1 N1 2.076(4) . ?
Cr1 N2 2.079(4) 15 ?
O1 C6 1.431(6) . ?
O2 C12 1.407(5) . ?
N1 C1 1.322(6) . ?
N1 C5 1.376(7) . ?
N2 C7 1.348(6) . ?
N2 C11 1.341(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.369(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.392(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(7) . ?
C5 C6 1.518(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.370(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.376(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.396(7) . ?
C11 C12 1.507(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Cl1 O3 1.381(7) 3_665 ?
Cl1 O3 1.381(7) . ?
Cl1 O3 1.381(7) 2_655 ?
Cl1 O3A 1.406(13) 3_665 ?
Cl1 O3A 1.406(13) . ?
Cl1 O3A 1.406(13) 2_655 ?
Cl1 O4 1.501(11) . ?
Cl1 O4A 1.468(15) . ?
Cl2 O5 1.404(7) . ?
Cl2 O6 1.426(7) 3_675 ?
Cl2 O6 1.426(7) . ?
Cl2 O6 1.426(7) 2_765 ?

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 Fe1 O1 82.90(16) . 14_455 ?
O1 Fe1 N1 79.38(14) . . ?
O1 Fe1 N2 157.77(14) . 15 ?
O2 Fe1 O1 76.23(12) . 14_455 ?
O2 Fe1 O1 78.35(12) 15 . ?
O2 Fe1 O1 93.00(12) 15 14_455 ?
O2 Fe1 O1 101.96(13) . . ?
O2 Fe1 O2 169.03(11) . 15 ?
O2 Fe1 N1 96.79(14) 15 . ?
O2 Fe1 N1 94.03(14) . . ?
O2 Fe1 N2 79.42(14) 15 15 ?
O2 Fe1 N2 99.83(14) . 15 ?
N1 Fe1 O1 157.55(14) . 14_455 ?
N1 Fe1 N2 103.47(15) . 15 ?
N2 Fe1 O1 98.16(13) 15 14_455 ?
O1 Fe2 O1 180.0 3_565 15 ?
O1 Fe2 O1 82.40(11) 2_665 15 ?
O1 Fe2 O1 82.40(11) . 15 ?
O1 Fe2 O1 180.00(15) . 13_565 ?
O1 Fe2 O1 82.40(11) 3_565 13_565 ?
O1 Fe2 O1 97.60(11) 15 14_455 ?
O1 Fe2 O1 82.40(11) 3_565 14_455 ?
O1 Fe2 O1 82.40(11) 2_665 13_565 ?
O1 Fe2 O1 97.61(11) 13_565 14_455 ?
O1 Fe2 O1 97.60(11) 2_665 3_565 ?
O1 Fe2 O1 97.60(11) . 3_565 ?
O1 Fe2 O1 180.0 2_665 14_455 ?
O1 Fe2 O1 97.60(11) 2_665 . ?
O1 Fe2 O1 82.40(11) . 14_455 ?
O1 Fe2 O1 97.60(11) 15 13_565 ?
O1 Cr1 O1 82.90(16) . 14_455 ?
O1 Cr1 N1 79.38(14) . . ?
O1 Cr1 N2 157.77(14) . 15 ?
O2 Cr1 O1 76.23(12) . 14_455 ?
O2 Cr1 O1 78.35(12) 15 . ?
O2 Cr1 O1 93.00(12) 15 14_455 ?
O2 Cr1 O1 101.96(13) . . ?
O2 Cr1 O2 169.03(11) . 15 ?
O2 Cr1 N1 96.79(14) 15 . ?
O2 Cr1 N1 94.03(14) . . ?
O2 Cr1 N2 79.42(14) 15 15 ?
O2 Cr1 N2 99.83(14) . 15 ?
N1 Cr1 O1 157.55(14) . 14_455 ?
N1 Cr1 N2 103.47(15) . 15 ?
N2 Cr1 O1 98.16(13) 15 14_455 ?
Fe1 O1 Fe1 97.92(12) . 15 ?
Fe1 O1 Fe2 98.69(13) . . ?
Fe2 O1 Fe1 95.80(12) . 15 ?
Cr1 O1 Fe2 98.69(13) . . ?
C6 O1 Fe1 112.4(3) . . ?
C6 O1 Fe1 119.0(3) . 15 ?
C6 O1 Fe2 127.5(2) . . ?
C6 O1 Cr1 112.4(3) . . ?
Fe1 O2 Fe1 107.48(15) . 14_455 ?
Cr1 O2 Fe1 107.48(15) . 14_455 ?
C12 O2 Fe1 133.7(3) . . ?
C12 O2 Fe1 118.8(3) . 14_455 ?
C12 O2 Cr1 133.7(3) . . ?
C1 N1 Fe1 128.0(4) . . ?
C1 N1 Cr1 128.0(4) . . ?
C1 N1 C5 118.2(5) . . ?
C5 N1 Fe1 113.9(3) . . ?
C5 N1 Cr1 113.9(3) . . ?
C7 N2 Fe1 126.9(4) . 14_455 ?
C11 N2 Fe1 114.9(3) . 14_455 ?
C11 N2 C7 118.1(4) . . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.4(6) . . ?
C2 C1 H1 118.3 . . ?
C1 C2 H2 120.5 . . ?
C1 C2 C3 119.1(6) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.5(6) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.3(5) . . ?
N1 C5 C6 115.9(4) . . ?
C4 C5 C6 122.7(5) . . ?
O1 C6 C5 110.0(4) . . ?
O1 C6 H6A 109.7 . . ?
O1 C6 H6B 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 H7 118.7 . . ?
N2 C7 C8 122.5(6) . . ?
C8 C7 H7 118.7 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.3(5) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.3(6) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 120.7 . . ?
C9 C10 C11 118.6(6) . . ?
C11 C10 H10 120.7 . . ?
N2 C11 C10 122.2(5) . . ?
N2 C11 C12 116.1(4) . . ?
C10 C11 C12 121.7(5) . . ?
O2 C12 C11 110.5(4) . . ?
O2 C12 H12A 109.6 . . ?
O2 C12 H12B 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
O3 Cl1 O3 114.8(4) 3_665 . ?
O3 Cl1 O3 114.8(4) 2_655 . ?
O3 Cl1 O3 114.8(4) 3_665 2_655 ?
O3 Cl1 O3A 121(2) 3_665 2_655 ?
O3 Cl1 O3A 27.2(12) 2_655 2_655 ?
O3 Cl1 O3A 121(2) . 3_665 ?
O3 Cl1 O3A 123(2) 2_655 3_665 ?
O3 Cl1 O3A 27.2(12) 3_665 3_665 ?
O3 Cl1 O3A 123(2) . 2_655 ?
O3 Cl1 O4 103.3(5) 3_665 . ?
O3 Cl1 O4 103.3(5) . . ?
O3 Cl1 O4 103.3(5) 2_655 . ?
O3A Cl1 O3A 114.5(9) 3_665 . ?
O3A Cl1 O3A 114.5(9) 3_665 2_655 ?
O3A Cl1 O3A 114.5(9) 2_655 . ?
O3A Cl1 O4A 103.8(12) 3_665 . ?
O3A Cl1 O4A 103.9(12) . . ?
O3A Cl1 O4A 103.8(12) 2_655 . ?
O5 Cl2 O6 110.7(4) . . ?
O5 Cl2 O6 110.7(4) . 3_675 ?
O5 Cl2 O6 110.7(4) . 2_765 ?
O6 Cl2 O6 108.2(4) 2_765 . ?
O6 Cl2 O6 108.2(4) 3_675 2_765 ?
O6 Cl2 O6 108.2(4) 3_675 . ?

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
Fe1 O1 C6 C5 -82.6(4) 15 . . . ?
Fe1 O1 C6 C5 30.9(4) . . . . ?
Fe1 O2 C12 C11 -4.3(6) 14_455 . . . ?
Fe1 O2 C12 C11 176.2(3) . . . . ?
Fe1 N1 C1 C2 -176.7(4) . . . . ?
Fe1 N1 C5 C4 176.5(4) . . . . ?
Fe1 N1 C5 C6 -2.1(5) . . . . ?
Fe1 N2 C7 C8 -175.0(4) 14_455 . . . ?
Fe1 N2 C11 C10 177.1(4) 14_455 . . . ?
Fe1 N2 C11 C12 -4.5(6) 14_455 . . . ?
Fe2 O1 C6 C5 152.5(3) . . . . ?
Cr1 O1 C6 C5 30.9(4) . . . . ?
Cr1 O2 C12 C11 176.2(3) . . . . ?
Cr1 N1 C1 C2 -176.7(4) . . . . ?
Cr1 N1 C5 C4 176.5(4) . . . . ?
Cr1 N1 C5 C6 -2.1(5) . . . . ?
N1 C1 C2 C3 0.4(9) . . . . ?
N1 C5 C6 O1 -19.0(6) . . . . ?
N2 C7 C8 C9 -0.9(9) . . . . ?
N2 C11 C12 O2 5.7(6) . . . . ?
C1 N1 C5 C4 -2.2(7) . . . . ?
C1 N1 C5 C6 179.3(4) . . . . ?
C1 C2 C3 C4 -2.2(10) . . . . ?
C2 C3 C4 C5 1.7(10) . . . . ?
C3 C4 C5 N1 0.5(9) . . . . ?
C3 C4 C5 C6 178.9(6) . . . . ?
C4 C5 C6 O1 162.5(5) . . . . ?
C5 N1 C1 C2 1.7(8) . . . . ?
C7 N2 C11 C10 1.5(7) . . . . ?
C7 N2 C11 C12 179.8(4) . . . . ?
C7 C8 C9 C10 0.2(10) . . . . ?
C8 C9 C10 C11 1.3(10) . . . . ?
C9 C10 C11 N2 -2.2(9) . . . . ?
C9 C10 C11 C12 179.5(6) . . . . ?
C10 C11 C12 O2 -176.0(5) . . . . ?
C11 N2 C7 C8 0.1(7) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-24
_olex2_date_sample_submission    2016-11-21
_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 788o
_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 2.009
_oxdiff_exptl_absorpt_empirical_full_min 0.575
_platon_squeeze_details          '9 MeOH per wheel'
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 472 151 ' '
2 -0.333 0.333 0.333 477 152 ' '
3 0.333 0.667 0.667 474 152 ' '

_platon_squeeze_void_probe_radius 1.20
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1855224'
_audit_update_record             
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
# local name eb16264
_audit_creation_date             2016-11-23
_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         
'C72 H72 Al2 Co5 N12 O12, 4(Cl1 O4), 9 (C H4 O)'
_chemical_formula_sum            'C81 H108 Al2 Cl4 Co5 N12 O37'
_chemical_formula_weight         2332.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C60 H100 N10 O30 Co6 Cl Al2'
_chemical_oxdiff_usercomment     '@ 120 K 756o'
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'
Al Al 0.0645 0.0514 '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'
Co Co 0.3494 0.9721 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   14.6812(5)
_cell_length_b                   14.6812(5)
_cell_length_c                   38.0235(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7097.5(5)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    12096
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      26.1220
_cell_measurement_theta_min      3.1830
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.710
_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 brown'
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3609
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 11 29 0.1378
-21 13 6 0.0267
20 -13 -8 0.0413
-5 -12 -30 0.1256
0 -1 5 0.0132
0 1 -5 0.0132

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.075
_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
5.9999 11.0001 28.9986 0.0059 -0.0749 0.9906
-20.9998 12.9997 5.9983 0.1830 -0.9937 -0.2019
19.9998 -12.9998 -7.9983 -0.1923 0.9627 0.1431
-5.0000 -12.0001 -29.9985 -0.0148 0.1315 -1.0043
0.0000 -1.0000 5.0000 0.1073 0.0156 0.0075
-0.0000 1.0000 -5.0000 -0.1073 -0.0156 -0.0075

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            38106
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.340
_diffrn_reflns_theta_max         25.340
_diffrn_reflns_theta_min         3.121
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
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   30.00    --   -9.43 -99.00  90.00   50
  2  ω    -80.00   5.00   1.00   30.00    --   -9.43 -57.00 150.00   85
  3  ω    -34.00  -5.00   1.00   30.00    --   -9.43  48.00 -80.39   29
  4  ω     21.00  48.00   1.00   30.00    --   10.84-140.00-170.98   27
  5  ω    -40.00 -13.00   1.00   30.00    --   10.84 -77.00 -90.00   27
  6  ω      0.00  27.00   1.00   30.00    --   10.84 -88.00 170.93   27
  7  ω    -40.00  42.00   1.00   30.00    --   10.84 -77.00-150.00   82
  8  ω     43.00  82.00   1.00   30.00    --   10.84  38.00-120.00   39
  9  ω    -45.00 -18.00   1.00   30.00    --   10.84 -38.00-150.00   27
 10  ω     24.00  51.00   1.00   30.00    --   10.84  38.00-150.00   27
 11  ω      2.00  65.00   1.00   30.00    --   10.84-124.00 102.42   63
 12  ω    -62.00  32.00   1.00   30.00    --   10.84 -38.00 -60.00   94
 13  ω    -37.00 -10.00   1.00   30.00    --   10.84 -77.00 120.00   27
 14  ω     38.00  65.00   1.00   30.00    --   10.84  19.00 -30.00   27
 15  ω     46.00  80.00   1.00   30.00    --   10.84  19.00 -60.00   34
;
_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      -0.0220616000
_diffrn_orient_matrix_UB_12      -0.0287998000
_diffrn_orient_matrix_UB_13      0.0156924000
_diffrn_orient_matrix_UB_21      0.0334685000
_diffrn_orient_matrix_UB_22      -0.0218039000
_diffrn_orient_matrix_UB_23      -0.0012383000
_diffrn_orient_matrix_UB_31      0.0387856000
_diffrn_orient_matrix_UB_32      0.0425051000
_diffrn_orient_matrix_UB_33      0.0100107000
_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                2560
_reflns_number_total             2893
_reflns_odcompleteness_completeness 99.83
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 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         0.728
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2893
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0623
_refine_ls_restrained_S_all      1.133
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0429P)²+68.7616P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1339
_refine_special_details          
;
The SQUEEZE routine of PLATON was used to account for electron density equivalent to 9 molecules of MeOH per wheel.  This missing solvent is included in the total chemical formula, triggering several checkCIF alerts which ought to be ignored.

One of the perchlorate anions was modelled as disordered over two sites, consistent with residual electron density.  Displacement ellipsoid and geometric similarity restraints were used.

One of the metal sites was modelled using substititional disorder between Co(II) and Al(III) in the ratio 5:2 per wheel.  This is consistent with charge balance requirements and other analytical data which support the 5:2 ratio.

 
#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
230_ALERT_2_C Hirshfeld Test Diff for    C8     --  C9      ..        5.2 s.u.
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0086 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      6.752 Check
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.125 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           5 Note

Not significant.

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          4 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          4 Report
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.2025 Check
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      68.76 Why ?
171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records          1 Report
176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          1 Report
187_ALERT_4_G The CIF-Embedded .res File Contains RIGU Records          1 Report
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  O1      ..        5.6 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  O2      ..        5.2 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  N2      ..        7.5 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  O1_i    ..        9.1 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Al1    --  O1      ..        5.6 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Al1    --  O2      ..        5.2 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Al1    --  N2      ..        7.5 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Al1    --  O1_i    ..        9.1 s.u.
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl1 Check
300_ALERT_4_G Atom Site Occupancy of >Co1    is Constrained at     0.6667 Check
300_ALERT_4_G Atom Site Occupancy of <Al1    is Constrained at     0.3333 Check
301_ALERT_3_G Main Residue  Disorder ............ Percentage =          4 Note
302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =         30 Note
605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        497 A**3


All of the above, which relate to the use of SQUEEZE or to disorder, are discussed above.

779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        124 Check
              O5   -CL2  -O5A     3.675   1.555   3.675             35.00 Deg.
779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        126 Check
              O5   -CL2  -O5A     2.765   1.555   2.765             35.00 Deg.
802_ALERT_4_G CIF Input Record(s) with more than 80 Characters          3 Info
860_ALERT_3_G Number of Least-Squares Restraints .............         18 Note
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note

Not significant


#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Co1, Al1}
3. Restrained distances
 Cl2-O5A \\sim Cl2-O5 \\sim Cl2-O6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Co1) = Uanis(Al1)
5. Rigid body (RIGU) restrains
 Cl2, O5, O5A, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O5A)=1-FVAR(1)
 Sof(O5)=FVAR(1)
 Fixed Sof: Co1(0.66666) Al1(0.33333)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     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
Co1 Co 0.76326(5) 0.82318(5) 0.49648(2) 0.0185(2) Uani 0.6667 1 d . . . A 1
Al1 Al 0.76326(5) 0.82318(5) 0.49648(2) 0.0185(2) Uani 0.3333 1 d . . . A 2
Co2 Co 1.000000 1.000000 0.500000 0.0206(3) Uani 1 6 d S T P A .
O1 O 0.8615(2) 0.9626(2) 0.47255(7) 0.0268(7) Uani 1 1 d . . . . .
O2 O 0.7338(2) 0.9205(2) 0.52387(8) 0.0317(8) Uani 1 1 d . . . . .
N1 N 0.6740(3) 0.8114(3) 0.45300(10) 0.0292(9) Uani 1 1 d . . . . .
N2 N 0.6492(3) 0.7190(3) 0.53021(10) 0.0307(9) Uani 1 1 d . . . . .
C1 C 0.5721(4) 0.7432(4) 0.44706(15) 0.0378(12) Uani 1 1 d . . . . .
H1 H 0.531724 0.695790 0.465265 0.045 Uiso 1 1 calc R . . . .
C2 C 0.5236(4) 0.7391(4) 0.41574(17) 0.0521(15) Uani 1 1 d . . . . .
H2 H 0.451068 0.689708 0.412497 0.063 Uiso 1 1 calc R . . . .
C3 C 0.5812(4) 0.8071(5) 0.38911(16) 0.0531(15) Uani 1 1 d . . . . .
H3 H 0.549511 0.804424 0.367049 0.064 Uiso 1 1 calc R . . . .
C4 C 0.6858(4) 0.8794(4) 0.39506(14) 0.0433(13) Uani 1 1 d . . . . .
H4 H 0.727086 0.927892 0.377220 0.052 Uiso 1 1 calc R . . . .
C5 C 0.7300(4) 0.8803(4) 0.42739(12) 0.0291(10) Uani 1 1 d . . . . .
C6 C 0.8438(3) 0.9575(4) 0.43579(12) 0.0294(10) Uani 1 1 d . . . . .
H6A H 0.889500 0.935454 0.423821 0.035 Uiso 1 1 calc R . . . .
H6B H 0.862178 1.028056 0.426913 0.035 Uiso 1 1 calc R . . . .
C7 C 0.6122(4) 0.6137(4) 0.53263(15) 0.0448(14) Uani 1 1 d . . . . .
H7 H 0.637057 0.581394 0.516614 0.054 Uiso 1 1 calc R . . . .
C8 C 0.5394(5) 0.5530(4) 0.55781(17) 0.0569(18) Uani 1 1 d . . . . .
H8 H 0.513906 0.479470 0.558697 0.068 Uiso 1 1 calc R . . . .
C9 C 0.5039(5) 0.5977(5) 0.58138(18) 0.0615(18) Uani 1 1 d . . . . .
H9 H 0.454686 0.556499 0.599066 0.074 Uiso 1 1 calc R . . . .
C10 C 0.5404(4) 0.7023(5) 0.57900(16) 0.0514(15) Uani 1 1 d . . . . .
H10 H 0.516102 0.734969 0.595092 0.062 Uiso 1 1 calc R . . . .
C11 C 0.6129(4) 0.7625(4) 0.55331(13) 0.0352(11) Uani 1 1 d . . . . .
C12 C 0.6553(4) 0.8784(4) 0.54925(13) 0.0370(12) Uani 1 1 d . . . . .
H12A H 0.597587 0.891217 0.542452 0.044 Uiso 1 1 calc R . . . .
H12B H 0.684126 0.913901 0.572035 0.044 Uiso 1 1 calc R . . . .
Cl1 Cl 0.333333 0.666667 0.50852(8) 0.0534(7) Uani 1 3 d S T P . .
O3 O 0.3633(3) 0.5928(3) 0.49881(15) 0.0725(14) Uani 1 1 d . . . . .
O4 O 0.333333 0.666667 0.5476(3) 0.112(4) Uani 1 3 d S T P . .
Cl2 Cl 1.000000 1.000000 0.34389(6) 0.0487(6) Uani 1 3 d DS TU P . .
O5 O 0.934(2) 0.8987(9) 0.3567(5) 0.089(6) Uani 0.59(6) 1 d D U . B 1
O6 O 1.000000 1.000000 0.30668(15) 0.0525(17) Uani 1 3 d DS TU P B .
O5A O 0.898(2) 0.929(5) 0.3554(8) 0.128(17) Uani 0.41(6) 1 d D U . B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.133(3) 12_656 ?
Co1 O1 2.036(3) . ?
Co1 O2 1.955(3) 12_656 ?
Co1 O2 1.982(3) . ?
Co1 N1 2.063(4) . ?
Co1 N2 2.056(4) . ?
Al1 O1 2.133(3) 12_656 ?
Al1 O1 2.036(3) . ?
Al1 O2 1.982(3) . ?
Al1 O2 1.955(3) 12_656 ?
Al1 N1 2.063(4) . ?
Al1 N2 2.056(4) . ?
Co2 O1 2.099(3) 10_776 ?
Co2 O1 2.099(3) 2_765 ?
Co2 O1 2.099(3) 12_656 ?
Co2 O1 2.099(3) 3_675 ?
Co2 O1 2.099(3) . ?
Co2 O1 2.099(3) 11_566 ?
O1 C6 1.417(5) . ?
O2 C12 1.389(5) . ?
N1 C1 1.339(6) . ?
N1 C5 1.348(6) . ?
N2 C7 1.361(6) . ?
N2 C11 1.343(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.373(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.376(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.382(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(7) . ?
C5 C6 1.511(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.379(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.359(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.354(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.388(7) . ?
C11 C12 1.500(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Cl1 O3 1.407(4) 3_565 ?
Cl1 O3 1.407(4) . ?
Cl1 O3 1.407(4) 2_665 ?
Cl1 O4 1.487(10) . ?
Cl2 O5 1.395(12) 2_765 ?
Cl2 O5 1.395(12) . ?
Cl2 O5 1.395(12) 3_675 ?
Cl2 O6 1.415(6) . ?
Cl2 O5A 1.405(12) 2_765 ?
Cl2 O5A 1.405(12) 3_675 ?
Cl2 O5A 1.405(13) . ?

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 Co1 O1 83.26(16) . 12_656 ?
O1 Co1 N1 80.06(14) . . ?
O1 Co1 N2 158.54(14) . . ?
O2 Co1 O1 79.06(13) . . ?
O2 Co1 O1 100.53(13) 12_656 . ?
O2 Co1 O1 77.35(12) 12_656 12_656 ?
O2 Co1 O1 91.76(13) . 12_656 ?
O2 Co1 O2 169.05(12) 12_656 . ?
O2 Co1 N1 93.62(14) 12_656 . ?
O2 Co1 N1 97.07(14) . . ?
O2 Co1 N2 100.79(15) 12_656 . ?
O2 Co1 N2 79.55(14) . . ?
N1 Co1 O1 159.25(14) . 12_656 ?
N2 Co1 O1 99.06(13) . 12_656 ?
N2 Co1 N1 100.99(15) . . ?
O1 Al1 O1 83.26(16) . 12_656 ?
O1 Al1 N1 80.06(14) . . ?
O1 Al1 N2 158.54(14) . . ?
O2 Al1 O1 100.53(13) 12_656 . ?
O2 Al1 O1 91.76(13) . 12_656 ?
O2 Al1 O1 77.35(12) 12_656 12_656 ?
O2 Al1 O1 79.06(13) . . ?
O2 Al1 O2 169.05(12) 12_656 . ?
O2 Al1 N1 97.07(14) . . ?
O2 Al1 N1 93.62(14) 12_656 . ?
O2 Al1 N2 79.55(14) . . ?
O2 Al1 N2 100.79(15) 12_656 . ?
N1 Al1 O1 159.25(14) . 12_656 ?
N2 Al1 O1 99.06(13) . 12_656 ?
N2 Al1 N1 100.99(15) . . ?
O1 Co2 O1 180.0 12_656 3_675 ?
O1 Co2 O1 97.43(10) 10_776 12_656 ?
O1 Co2 O1 82.57(10) 10_776 2_765 ?
O1 Co2 O1 97.43(10) 2_765 3_675 ?
O1 Co2 O1 97.43(10) 11_566 12_656 ?
O1 Co2 O1 180.00(13) 11_566 2_765 ?
O1 Co2 O1 82.57(10) 2_765 12_656 ?
O1 Co2 O1 82.57(10) . 11_566 ?
O1 Co2 O1 97.43(10) 10_776 11_566 ?
O1 Co2 O1 82.57(10) 10_776 3_675 ?
O1 Co2 O1 97.43(10) . 3_675 ?
O1 Co2 O1 82.57(10) . 12_656 ?
O1 Co2 O1 82.57(10) 11_566 3_675 ?
O1 Co2 O1 180.0 . 10_776 ?
O1 Co2 O1 97.43(10) . 2_765 ?
Co1 O1 Co1 97.76(12) . 11_566 ?
Co1 O1 Co2 98.47(12) . . ?
Al1 O1 Co2 98.47(12) . . ?
Co2 O1 Co1 95.51(12) . 11_566 ?
C6 O1 Co1 111.6(3) . . ?
C6 O1 Co1 118.5(3) . 11_566 ?
C6 O1 Al1 111.6(3) . . ?
C6 O1 Co2 129.3(3) . . ?
Co1 O2 Co1 105.83(14) 11_566 . ?
C12 O2 Co1 118.4(3) . . ?
C12 O2 Co1 135.5(3) . 11_566 ?
C12 O2 Al1 118.4(3) . . ?
C1 N1 Co1 128.6(3) . . ?
C1 N1 Al1 128.6(3) . . ?
C1 N1 C5 118.3(4) . . ?
C5 N1 Co1 113.1(3) . . ?
C5 N1 Al1 113.1(3) . . ?
C7 N2 Co1 126.9(4) . . ?
C7 N2 Al1 126.9(4) . . ?
C11 N2 Co1 115.1(3) . . ?
C11 N2 Al1 115.1(3) . . ?
C11 N2 C7 117.9(5) . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.7(5) . . ?
C2 C1 H1 118.7 . . ?
C1 C2 H2 120.3 . . ?
C1 C2 C3 119.3(5) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.7(5) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.2(5) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.8(4) . . ?
N1 C5 C6 116.2(4) . . ?
C4 C5 C6 122.1(4) . . ?
O1 C6 C5 110.7(4) . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6B 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N2 C7 H7 119.3 . . ?
N2 C7 C8 121.4(6) . . ?
C8 C7 H7 119.3 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.4(5) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 120.9 . . ?
C10 C9 C8 118.3(6) . . ?
C10 C9 H9 120.9 . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 120.8(6) . . ?
C11 C10 H10 119.6 . . ?
N2 C11 C10 121.2(5) . . ?
N2 C11 C12 115.7(4) . . ?
C10 C11 C12 123.1(5) . . ?
O2 C12 C11 111.0(4) . . ?
O2 C12 H12A 109.4 . . ?
O2 C12 H12B 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
O3 Cl1 O3 113.4(2) 3_565 . ?
O3 Cl1 O3 113.4(2) 3_565 2_665 ?
O3 Cl1 O3 113.4(2) 2_665 . ?
O3 Cl1 O4 105.2(3) . . ?
O3 Cl1 O4 105.2(3) 3_565 . ?
O3 Cl1 O4 105.2(3) 2_665 . ?
O5 Cl2 O5 108.4(8) 3_675 2_765 ?
O5 Cl2 O5 108.4(8) . 2_765 ?
O5 Cl2 O5 108.4(8) 3_675 . ?
O5 Cl2 O6 110.5(8) 3_675 . ?
O5 Cl2 O6 110.5(8) 2_765 . ?
O5 Cl2 O6 110.5(8) . . ?
O5 Cl2 O5A 35(2) 2_765 2_765 ?
O5 Cl2 O5A 35(2) 3_675 3_675 ?
O5 Cl2 O5A 76.9(19) . 2_765 ?
O5 Cl2 O5A 135.5(17) 3_675 2_765 ?
O5 Cl2 O5A 76.9(19) 2_765 3_675 ?
O5 Cl2 O5A 135.5(17) . 3_675 ?
O5A Cl2 O6 108.1(13) . . ?
O5A Cl2 O6 108.1(13) 3_675 . ?
O5A Cl2 O6 108.1(13) 2_765 . ?
O5A Cl2 O5A 110.8(12) 3_675 . ?
O5A Cl2 O5A 110.8(12) . 2_765 ?
O5A Cl2 O5A 110.8(13) 3_675 2_765 ?

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
Co1 O1 C6 C5 30.2(4) . . . . ?
Co1 O1 C6 C5 -82.1(4) 11_566 . . . ?
Co1 O2 C12 C11 178.9(3) 11_566 . . . ?
Co1 O2 C12 C11 5.4(5) . . . . ?
Co1 N1 C1 C2 -175.3(4) . . . . ?
Co1 N1 C5 C4 175.1(4) . . . . ?
Co1 N1 C5 C6 -4.2(5) . . . . ?
Co1 N2 C7 C8 176.3(4) . . . . ?
Co1 N2 C11 C10 -176.1(4) . . . . ?
Co1 N2 C11 C12 4.2(5) . . . . ?
Al1 O1 C6 C5 30.2(4) . . . . ?
Al1 O2 C12 C11 5.4(5) . . . . ?
Al1 N1 C1 C2 -175.3(4) . . . . ?
Al1 N1 C5 C4 175.1(4) . . . . ?
Al1 N1 C5 C6 -4.2(5) . . . . ?
Al1 N2 C7 C8 176.3(4) . . . . ?
Al1 N2 C11 C10 -176.1(4) . . . . ?
Al1 N2 C11 C12 4.2(5) . . . . ?
Co2 O1 C6 C5 152.1(3) . . . . ?
N1 C1 C2 C3 0.2(9) . . . . ?
N1 C5 C6 O1 -17.2(6) . . . . ?
N2 C7 C8 C9 -1.1(8) . . . . ?
N2 C11 C12 O2 -6.1(6) . . . . ?
C1 N1 C5 C4 -2.4(7) . . . . ?
C1 N1 C5 C6 178.4(4) . . . . ?
C1 C2 C3 C4 -1.5(9) . . . . ?
C2 C3 C4 C5 0.9(9) . . . . ?
C3 C4 C5 N1 1.1(8) . . . . ?
C3 C4 C5 C6 -179.7(5) . . . . ?
C4 C5 C6 O1 163.5(4) . . . . ?
C5 N1 C1 C2 1.8(7) . . . . ?
C7 N2 C11 C10 0.4(7) . . . . ?
C7 N2 C11 C12 -179.4(4) . . . . ?
C7 C8 C9 C10 1.2(9) . . . . ?
C8 C9 C10 C11 -0.5(9) . . . . ?
C9 C10 C11 N2 -0.2(9) . . . . ?
C9 C10 C11 C12 179.5(5) . . . . ?
C10 C11 C12 O2 174.1(5) . . . . ?
C11 N2 C7 C8 0.3(7) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-17
_olex2_date_sample_submission    2016-10-14
_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 '756o 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 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.737
_vrf_CHEMW03_5                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Please see the _refine_special_details section of the CIF
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1855223'
_audit_update_record             
;
2018-07-11 deposited with the CCDC.
2018-10-15 downloaded from the CCDC.
;
# local name eb16213
_audit_creation_date             2016-09-07
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H72 Co5 Cr2 N12 O12, 4(Cl1 O4), 9 C H4 O'
_chemical_formula_sum            'C81 H108 Cl4 Co5 Cr2 N12 O37'
_chemical_formula_weight         2382.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Cr Cl Co'
_chemical_oxdiff_usercomment     '@ 120 K 698o'
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'
Co Co 0.3494 0.9721 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   14.7268(2)
_cell_length_b                   14.7268(2)
_cell_length_c                   38.1319(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7162.0(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    26180
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.9710
_cell_measurement_theta_min      3.1880
_shelx_estimated_absorpt_T_max   0.883
_shelx_estimated_absorpt_T_min   0.685
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0659 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.9174.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark pink'
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3675
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-17 15 22 0.0492
-7 -13 11 0.1000
7 13 -12 0.0623
-15 17 25 0.0480
-9 -10 16 0.0984
-12 -6 -23 0.0661
13 3 31 0.0886
8 -10 47 0.0950
-11 5 -45 0.0918
13 -17 -28 0.0704
-1 -2 -53 0.0756
5 11 -32 0.0646
14 -20 -5 0.0506
-3 5 52 0.0641
-20 4 -2 0.0610
0 17 -14 0.0549
4 2 52 0.0706

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.1
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
-17.0000 15.0001 22.0002 -0.8574 -0.4830 -0.0202
-7.0000 -13.0001 11.0004 -0.0166 0.0127 -0.9983
7.0000 13.0001 -12.0004 0.0151 0.0054 1.0024
-15.0000 17.0001 25.0002 -0.8141 -0.5757 0.1523
-9.0000 -10.0000 16.0005 -0.1355 -0.1037 -0.9472
-12.0000 -6.0000 -23.0003 -0.3711 0.5697 -0.7073
13.0000 3.0000 31.0005 0.4716 -0.6822 0.5623
8.0000 -10.0000 47.0010 0.5359 -0.7728 -0.3741
-11.0000 5.0000 -45.0009 -0.5568 0.8200 -0.0134
13.0000 -17.0001 -28.0003 0.7360 0.6427 -0.2223
-1.0000 -2.0000 -53.0009 -0.0772 0.9912 0.0718
5.0000 11.0000 -32.0008 -0.0522 0.4058 0.8990
14.0000 -20.0001 -4.9998 0.8577 0.2587 -0.4283
-3.0000 5.0001 52.0009 -0.1241 -0.9863 -0.0785
-20.0000 4.0000 -2.0001 -0.8107 0.1119 -0.6094
0.0000 17.0001 -14.0005 -0.3157 0.0347 0.9275
4.0000 2.0000 52.0009 0.1865 -0.9922 0.0557

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            43856
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.648
_diffrn_reflns_theta_min         3.112
_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 0.939
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -88.00 -44.00   1.00   15.00    --   -9.43 162.00 167.05   44
  2  ω    -20.00  30.00   1.00   15.00    --   -9.43 -99.00  60.00   50
  3  ω    -46.00  69.00   1.00   15.00    --   -9.43  19.00-120.00  115
  4  ω    -41.00  64.00   1.00   15.00    --   -9.43  77.00  90.00  105
  5  ω    -20.00  15.00   1.00   15.00    --   -9.43 -99.00 150.00   35
  6  ω    -37.00 -10.00   1.00   15.00    --   -9.43  77.00 -60.00   27
  7  ω     16.00  42.00   1.00   15.00    --   -9.43  77.00 -60.00   26
  8  ω    -19.00  29.00   1.00   15.00    --   -9.43 -99.00-180.00   48
  9  ω    -20.00   5.00   1.00   15.00    --   -9.43 -99.00 -60.00   25
 10  ω    -30.00  -3.00   1.00   15.00    --   10.84 -38.00 150.00   27
 11  ω     25.00  50.00   1.00   15.00    --   10.84 -99.00-150.00   25
 12  ω     24.00  84.00   1.00   15.00    --   10.84-153.00  76.73   60
 13  ω     34.00  61.00   1.00   15.00    --   10.84-160.00 -67.34   27
 14  ω     -5.00  22.00   1.00   15.00    --   10.84-116.00-154.34   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      0.0369109000
_diffrn_orient_matrix_UB_12      -0.0174025000
_diffrn_orient_matrix_UB_13      0.0014169000
_diffrn_orient_matrix_UB_21      -0.0063580000
_diffrn_orient_matrix_UB_22      -0.0128628000
_diffrn_orient_matrix_UB_23      -0.0180966000
_diffrn_orient_matrix_UB_31      0.0411202000
_diffrn_orient_matrix_UB_32      0.0512150000
_diffrn_orient_matrix_UB_33      -0.0040626000
_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                3674
_reflns_number_total             4234
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4234
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0425
_refine_ls_restrained_S_all      1.068
_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)+(0.0173P)²+27.2577P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0914
_refine_special_details          
;
One of the perchlorate anions was modelled with three of the four oxygen atoms disordered over two positions.  Displacement ellipsoid and geometric similarity restraints were used.  The occupancies of Co1/Cr1, which exhibit subsitutional disorder, were fixed at a ratio of 2:1 for the purpose of correct charge balance.  Electron density pertaining to nine molecules of methanol was handled using the SQUEEZE routine of PLATON.  This extra solvent was included in the total formula, triggering checkCIF alerts, which should be ignored.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
906_ALERT_3_C Large K value in the Analysis of Variance ......      3.228 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min)           5 Note

Not significant.  Disorder of one perchlorate.

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          4 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          4 Report
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.2006 Check
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      27.26 Why ?
171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records          1 Report
176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          1 Report
187_ALERT_4_G The CIF-Embedded .res File Contains RIGU Records          1 Report
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  O1      ..        6.1 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  N1      ..        5.4 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  O1_h    ..        7.9 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Co1    --  N2_i    ..        6.2 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  O1      ..        6.1 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  N1      ..        5.4 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  O1_h    ..        7.9 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cr1    --  N2_i    ..        6.2 s.u.
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl1 Check
300_ALERT_4_G Atom Site Occupancy of >Co1    is Constrained at     0.6667 Check
300_ALERT_4_G Atom Site Occupancy of <Cr1    is Constrained at     0.3333 Check
301_ALERT_3_G Main Residue  Disorder ............ Percentage =          4 Note
302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =         30 Note
605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        510 A**3
764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.13 Ratio
860_ALERT_3_G Number of Least-Squares Restraints .............         18 Note
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600        252 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

None of the above are significant issues.  One perchlorate anion was modelled as disordered, and SQUEEZE was used.  Both of these are discussed above.

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Co1, Cr1}
3. Restrained distances
 Cl2-O5 \\sim Cl2-O6 \\sim Cl2-O6A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Co1) = Uanis(Cr1)
5. Rigid body (RIGU) restrains
 Cl2, O5, O6, O6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O6A)=1-FVAR(1)
 Sof(O6)=FVAR(1)
 Fixed Sof: Co1(0.66666) Cr1(0.33333)
7.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     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
Co1 Co 0.82236(2) 0.76298(2) 0.50334(2) 0.01818(9) Uani 0.6667 1 d . . . A 1
Cr1 Cr 0.82236(2) 0.76298(2) 0.50334(2) 0.01818(9) Uani 0.3333 1 d . . . A 2
Co2 Co 1.0000 1.0000 0.5000 0.01729(14) Uani 1 6 d S T P A .
O1 O 0.96234(11) 0.86205(11) 0.52779(4) 0.0212(3) Uani 1 1 d . . . . .
O2 O 0.73297(11) 0.81394(11) 0.52470(4) 0.0242(3) Uani 1 1 d . . . . .
N1 N 0.81183(13) 0.67353(13) 0.54706(5) 0.0217(4) Uani 1 1 d . . . . .
N2 N 0.64775(14) 0.93172(14) 0.53034(5) 0.0242(4) Uani 1 1 d . . . . .
C1 C 0.74364(18) 0.57116(17) 0.55254(7) 0.0296(5) Uani 1 1 d . . . . .
H1 H 0.6970 0.5310 0.5342 0.035 Uiso 1 1 calc R . . . .
C2 C 0.7395(2) 0.5228(2) 0.58401(8) 0.0398(6) Uani 1 1 d . . . . .
H2 H 0.6904 0.4505 0.5873 0.048 Uiso 1 1 calc R . . . .
C3 C 0.8069(2) 0.5804(2) 0.61049(8) 0.0448(7) Uani 1 1 d . . . . .
H3 H 0.8042 0.5487 0.6325 0.054 Uiso 1 1 calc R . . . .
C4 C 0.8790(2) 0.6853(2) 0.60478(7) 0.0358(6) Uani 1 1 d . . . . .
H4 H 0.9273 0.7262 0.6226 0.043 Uiso 1 1 calc R . . . .
C5 C 0.87970(17) 0.72970(16) 0.57256(6) 0.0230(4) Uani 1 1 d . . . . .
C6 C 0.95601(17) 0.84359(16) 0.56441(5) 0.0226(4) Uani 1 1 d . . . . .
H6A H 0.9329 0.8884 0.5763 0.027 Uiso 1 1 calc R . . . .
H6B H 1.0263 0.8626 0.5735 0.027 Uiso 1 1 calc R . . . .
C7 C 0.61195(19) 0.9998(2) 0.53249(7) 0.0325(5) Uani 1 1 d . . . . .
H7 H 0.6371 1.0561 0.5162 0.039 Uiso 1 1 calc R . . . .
C8 C 0.5402(2) 0.9904(2) 0.55748(8) 0.0421(7) Uani 1 1 d . . . . .
H8 H 0.5160 1.0393 0.5583 0.051 Uiso 1 1 calc R . . . .
C9 C 0.5039(2) 0.9092(2) 0.58117(8) 0.0456(7) Uani 1 1 d . . . . .
H9 H 0.4547 0.9017 0.5987 0.055 Uiso 1 1 calc R . . . .
C10 C 0.5395(2) 0.8391(2) 0.57931(7) 0.0382(6) Uani 1 1 d . . . . .
H10 H 0.5150 0.7824 0.5954 0.046 Uiso 1 1 calc R . . . .
C11 C 0.61183(17) 0.85208(17) 0.55355(6) 0.0261(5) Uani 1 1 d . . . . .
C12 C 0.65276(19) 0.77680(18) 0.54954(6) 0.0298(5) Uani 1 1 d . . . . .
H12A H 0.6795 0.7683 0.5724 0.036 Uiso 1 1 calc R . . . .
H12B H 0.5949 0.7073 0.5422 0.036 Uiso 1 1 calc R . . . .
Cl1 Cl 0.3333 0.6667 0.50932(3) 0.0376(2) Uani 1 3 d S T P . .
O3 O 0.3333 0.6667 0.54762(12) 0.0786(14) Uani 1 3 d S T P . .
O4 O 0.40630(15) 0.63611(16) 0.49811(7) 0.0520(6) Uani 1 1 d . . . . .
Cl2 Cl 1.0000 1.0000 0.65637(3) 0.0390(3) Uani 1 3 d DS TU P . .
O5 O 1.0000 1.0000 0.69372(8) 0.0399(7) Uani 1 3 d DS TU P B .
O6 O 0.8979(5) 0.9331(16) 0.6426(2) 0.075(4) Uani 0.49(3) 1 d D U . B 1
O6A O 0.9331(19) 0.8965(8) 0.6448(2) 0.093(8) Uani 0.51(3) 1 d D U . B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.1513(15) 11_566 ?
Co1 O1 2.0591(15) . ?
Co1 O2 1.9868(14) . ?
Co1 O2 1.9986(15) 12_656 ?
Co1 N1 2.0821(18) . ?
Co1 N2 2.0794(19) 12_656 ?
Cr1 O1 2.0591(15) . ?
Cr1 O1 2.1513(15) 11_566 ?
Cr1 O2 1.9868(14) . ?
Cr1 O2 1.9986(15) 12_656 ?
Cr1 N1 2.0821(18) . ?
Cr1 N2 2.0794(19) 12_656 ?
Co2 O1 2.1049(14) 12_656 ?
Co2 O1 2.1049(14) 2_765 ?
Co2 O1 2.1049(14) 10_776 ?
Co2 O1 2.1049(14) 11_566 ?
Co2 O1 2.1050(14) . ?
Co2 O1 2.1049(14) 3_675 ?
O1 Co1 2.1514(15) 12_656 ?
O1 Cr1 2.1514(15) 12_656 ?
O1 C6 1.417(3) . ?
O2 Co1 1.9986(15) 11_566 ?
O2 Cr1 1.9986(15) 11_566 ?
O2 C12 1.395(3) . ?
N1 C1 1.346(3) . ?
N1 C5 1.342(3) . ?
N2 Co1 2.0793(18) 11_566 ?
N2 Cr1 2.0793(18) 11_566 ?
N2 C7 1.348(3) . ?
N2 C11 1.348(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.381(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.372(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.386(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(3) . ?
C5 C6 1.513(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.378(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.375(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.390(3) . ?
C11 C12 1.511(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Cl1 O3 1.460(5) . ?
Cl1 O4 1.422(2) 3_565 ?
Cl1 O4 1.422(2) 2_665 ?
Cl1 O4 1.422(2) . ?
Cl2 O5 1.424(3) . ?
Cl2 O6 1.424(7) 2_765 ?
Cl2 O6 1.424(7) . ?
Cl2 O6 1.424(7) 3_675 ?
Cl2 O6A 1.410(6) . ?
Cl2 O6A 1.410(5) 2_765 ?
Cl2 O6A 1.410(5) 3_675 ?

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 Co1 O1 83.07(8) . 11_566 ?
O1 Co1 N1 79.46(6) . . ?
O1 Co1 N2 159.48(7) . 12_656 ?
O2 Co1 O1 80.07(6) 12_656 . ?
O2 Co1 O1 99.46(6) . . ?
O2 Co1 O1 78.11(6) . 11_566 ?
O2 Co1 O1 91.24(6) 12_656 11_566 ?
O2 Co1 O2 169.29(6) . 12_656 ?
O2 Co1 N1 97.15(7) 12_656 . ?
O2 Co1 N1 93.25(7) . . ?
O2 Co1 N2 79.53(7) 12_656 12_656 ?
O2 Co1 N2 100.99(7) . 12_656 ?
N1 Co1 O1 158.97(6) . 11_566 ?
N2 Co1 O1 99.46(6) 12_656 11_566 ?
N2 Co1 N1 101.00(7) 12_656 . ?
O1 Cr1 O1 83.07(8) . 11_566 ?
O1 Cr1 N1 79.46(6) . . ?
O1 Cr1 N2 159.48(7) . 12_656 ?
O2 Cr1 O1 99.46(6) . . ?
O2 Cr1 O1 91.24(6) 12_656 11_566 ?
O2 Cr1 O1 78.11(6) . 11_566 ?
O2 Cr1 O1 80.07(6) 12_656 . ?
O2 Cr1 O2 169.29(6) . 12_656 ?
O2 Cr1 N1 93.25(7) . . ?
O2 Cr1 N1 97.15(7) 12_656 . ?
O2 Cr1 N2 100.99(7) . 12_656 ?
O2 Cr1 N2 79.53(7) 12_656 12_656 ?
N1 Cr1 O1 158.97(6) . 11_566 ?
N2 Cr1 O1 99.46(6) 12_656 11_566 ?
N2 Cr1 N1 101.00(7) 12_656 . ?
O1 Co2 O1 96.88(5) 2_765 . ?
O1 Co2 O1 83.12(5) 12_656 . ?
O1 Co2 O1 180.00(7) 12_656 3_675 ?
O1 Co2 O1 96.89(5) 10_776 12_656 ?
O1 Co2 O1 83.12(5) 11_566 . ?
O1 Co2 O1 83.11(5) 11_566 3_675 ?
O1 Co2 O1 180.0 10_776 . ?
O1 Co2 O1 96.89(5) 11_566 10_776 ?
O1 Co2 O1 96.89(5) 11_566 12_656 ?
O1 Co2 O1 96.88(5) 3_675 . ?
O1 Co2 O1 83.11(5) 2_765 12_656 ?
O1 Co2 O1 180.0 11_566 2_765 ?
O1 Co2 O1 83.11(5) 2_765 10_776 ?
O1 Co2 O1 96.89(5) 2_765 3_675 ?
O1 Co2 O1 83.11(5) 10_776 3_675 ?
Co1 O1 Co1 97.08(6) . 12_656 ?
Co1 O1 Co2 98.23(6) . . ?
Cr1 O1 Cr1 97.08(6) . 12_656 ?
Cr1 O1 Co2 98.23(6) . . ?
Co2 O1 Co1 95.40(6) . 12_656 ?
Co2 O1 Cr1 95.40(6) . 12_656 ?
C6 O1 Co1 111.34(12) . . ?
C6 O1 Co1 118.72(12) . 12_656 ?
C6 O1 Cr1 111.34(12) . . ?
C6 O1 Cr1 118.72(12) . 12_656 ?
C6 O1 Co2 129.92(12) . . ?
Co1 O2 Co1 104.73(7) . 11_566 ?
Cr1 O2 Cr1 104.73(7) . 11_566 ?
C12 O2 Co1 118.55(13) . 11_566 ?
C12 O2 Co1 136.18(13) . . ?
C12 O2 Cr1 118.55(13) . 11_566 ?
C12 O2 Cr1 136.18(13) . . ?
C1 N1 Co1 127.65(16) . . ?
C1 N1 Cr1 127.65(16) . . ?
C5 N1 Co1 113.15(14) . . ?
C5 N1 Cr1 113.15(14) . . ?
C5 N1 C1 119.1(2) . . ?
C7 N2 Co1 126.94(17) . 11_566 ?
C7 N2 Cr1 126.94(17) . 11_566 ?
C7 N2 C11 118.5(2) . . ?
C11 N2 Co1 114.40(14) . 11_566 ?
C11 N2 Cr1 114.40(14) . 11_566 ?
N1 C1 H1 119.1 . . ?
N1 C1 C2 121.9(2) . . ?
C2 C1 H1 119.1 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.3(2) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.2(2) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(2) . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 121.5(2) . . ?
N1 C5 C6 116.49(18) . . ?
C4 C5 C6 122.0(2) . . ?
O1 C6 C5 110.88(17) . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6B 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N2 C7 H7 118.9 . . ?
N2 C7 C8 122.2(2) . . ?
C8 C7 H7 118.9 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.1(2) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.4(2) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 120.4 . . ?
C9 C10 C11 119.2(3) . . ?
C11 C10 H10 120.4 . . ?
N2 C11 C10 121.6(2) . . ?
N2 C11 C12 116.41(19) . . ?
C10 C11 C12 122.0(2) . . ?
O2 C12 C11 110.56(18) . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
O4 Cl1 O3 107.49(11) 2_665 . ?
O4 Cl1 O3 107.49(11) . . ?
O4 Cl1 O3 107.49(11) 3_565 . ?
O4 Cl1 O4 111.38(10) 3_565 . ?
O4 Cl1 O4 111.38(10) 2_665 . ?
O4 Cl1 O4 111.38(10) 2_665 3_565 ?
O6 Cl2 O5 111.7(3) 2_765 . ?
O6 Cl2 O5 111.7(3) 3_675 . ?
O6 Cl2 O5 111.7(3) . . ?
O6 Cl2 O6 107.2(3) 3_675 . ?
O6 Cl2 O6 107.2(3) 2_765 . ?
O6 Cl2 O6 107.2(4) 3_675 2_765 ?
O6A Cl2 O5 108.3(4) 3_675 . ?
O6A Cl2 O5 108.3(4) . . ?
O6A Cl2 O5 108.3(4) 2_765 . ?
O6A Cl2 O6A 110.6(4) 3_675 . ?
O6A Cl2 O6A 110.6(4) 3_675 2_765 ?
O6A Cl2 O6A 110.6(4) . 2_765 ?

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
Co1 O1 C6 C5 30.8(2) . . . . ?
Co1 O1 C6 C5 -80.66(18) 12_656 . . . ?
Co1 O2 C12 C11 -177.51(15) . . . . ?
Co1 O2 C12 C11 -7.5(3) 11_566 . . . ?
Co1 N1 C1 C2 -174.74(18) . . . . ?
Co1 N1 C5 C4 175.15(18) . . . . ?
Co1 N1 C5 C6 -4.4(2) . . . . ?
Co1 N2 C7 C8 -175.45(19) 11_566 . . . ?
Co1 N2 C11 C10 175.91(19) 11_566 . . . ?
Co1 N2 C11 C12 -5.3(3) 11_566 . . . ?
Cr1 O1 C6 C5 30.8(2) . . . . ?
Cr1 O1 C6 C5 -80.66(18) 12_656 . . . ?
Cr1 O2 C12 C11 -177.51(15) . . . . ?
Cr1 O2 C12 C11 -7.5(3) 11_566 . . . ?
Cr1 N1 C1 C2 -174.74(18) . . . . ?
Cr1 N1 C5 C4 175.15(18) . . . . ?
Cr1 N1 C5 C6 -4.4(2) . . . . ?
Cr1 N2 C7 C8 -175.45(19) 11_566 . . . ?
Cr1 N2 C11 C10 175.91(19) 11_566 . . . ?
Cr1 N2 C11 C12 -5.3(3) 11_566 . . . ?
Co2 O1 C6 C5 152.58(13) . . . . ?
N1 C1 C2 C3 -0.3(4) . . . . ?
N1 C5 C6 O1 -17.5(3) . . . . ?
N2 C7 C8 C9 0.3(4) . . . . ?
N2 C11 C12 O2 8.2(3) . . . . ?
C1 N1 C5 C4 -1.9(3) . . . . ?
C1 N1 C5 C6 178.52(19) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C2 C3 C4 C5 1.2(4) . . . . ?
C3 C4 C5 N1 0.4(4) . . . . ?
C3 C4 C5 C6 180.0(2) . . . . ?
C4 C5 C6 O1 162.9(2) . . . . ?
C5 N1 C1 C2 1.8(3) . . . . ?
C7 N2 C11 C10 0.0(3) . . . . ?
C7 N2 C11 C12 178.8(2) . . . . ?
C7 C8 C9 C10 -0.4(4) . . . . ?
C8 C9 C10 C11 0.3(4) . . . . ?
C9 C10 C11 N2 -0.1(4) . . . . ?
C9 C10 C11 C12 -178.8(2) . . . . ?
C10 C11 C12 O2 -173.0(2) . . . . ?
C11 N2 C7 C8 -0.1(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-24
_olex2_date_sample_submission    2016-08-19
_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 698o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.135
_oxdiff_exptl_absorpt_empirical_full_min 0.910
_vrf_CHEMW03_1                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: Please see the _refine_special_details section of the CIF.
;
