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

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1819131'
_audit_update_record             
;
2018-01-24 deposited with the CCDC.
2018-03-15 downloaded from the CCDC.
;
# local name eb16125
_audit_creation_date             2016-04-20
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C72 H72 Cr2 N12 Ni5 O12, 4(Cl1 O4), 3.5 C H4 O'
_chemical_formula_sum            'C79 H100 Cl4 Cr2 N12 Ni5 O35'
_chemical_formula_weight         2317.05
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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                   14.6131(3)
_cell_length_b                   14.6131(3)
_cell_length_c                   37.2857(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6895.4(3)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    7987
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.181
_cell_measurement_theta_min      2.714
_shelx_estimated_absorpt_T_max   0.870
_shelx_estimated_absorpt_T_min   0.654
_exptl_absorpt_coefficient_mu    1.439
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0665 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.7879.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3582
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            26509
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.339
_diffrn_reflns_theta_min         1.638
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEXII diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   Mo
_diffrn_source_current           30
_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                2044
_reflns_number_total             2823
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       APE2
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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         0.976
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0548
_refine_ls_restrained_S_all      1.086
_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)+(0.0985P)²+35.3976P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1752
_refine_special_details          
;The site of Ni1 was modelled as a 2/1 disorder with chromium.  Effectively this amounts to a disorder of two Cr per six outer Ni sites in the ring, and is consistent with bond valence calculations and charge balance considerations.  Ni2 was modelled as whollly nickel on the basis of BVS calculations.

The SQUEEZE routine of PLATON was used to account for 3.5 molecules of methanol per asymmetric unit.  This solvent is included in the total formula, triggering several 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
 
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0084 Ang.
905_ALERT_3_C Negative K value in the Analysis of Variance ...     -3.875 Report
924_ALERT_1_C The Reported and Calculated Rho(min) Differ by .       1.23 eA-3

Not significant

#===============================================================================
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.1621 Check
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check

All a consequence of SQUEEZE

083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      35.39 Why ?
171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records          1 Report
244_ALERT_4_G Low   'Solvent' Ueq as Compared to Neighbors of         Cl1 Check
244_ALERT_4_G Low   'Solvent' Ueq as Compared to Neighbors of         Cl2 Check
300_ALERT_4_G Atom Site Occupancy of >Ni1    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
605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        459 A**3
760_ALERT_1_G CIF Contains no Torsion Angles .................          ? Info
802_ALERT_4_G CIF Input Record(s) with more than 80 Characters          2 Info
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
#===============================================================================,SQUEEZE
;

# SQUEEZE RESULTS (Version =  11015)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 461 107 ' '
2 -0.333 0.333 0.333 463 108 ' '
3 0.333 0.667 0.667 463 107 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          '3.5 MeOH per asymmetric unit'




_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Ni1, Cr1}
3. Uiso/Uaniso restraints and constraints
Uanis(Ni1) = Uanis(Cr1)
4. Others
 Fixed Sof: Ni1(0.66666) Cr1(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(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.23781(5) 0.17471(5) 0.50268(2) 0.0353(2) Uani 0.6667 1 d . . . A 1
Ni2 Ni 0.0000 0.0000 0.5000 0.0351(4) Uani 1 6 d S T P A .
Cr1 Cr 0.23781(5) 0.17471(5) 0.50268(2) 0.0353(2) Uani 0.3333 1 d . . . A 2
O1 O 0.1371(2) 0.0358(2) 0.52758(9) 0.0347(7) Uani 1 1 d . . . . .
O2 O 0.2671(3) 0.0779(2) 0.47475(9) 0.0430(8) Uani 1 1 d . . . . .
N1 N 0.3267(3) 0.1870(3) 0.54677(11) 0.0452(10) Uani 1 1 d . . . . .
N2 N 0.3497(3) 0.2825(3) 0.46906(11) 0.0421(9) Uani 1 1 d . . . . .
C1 C 0.4284(4) 0.2551(4) 0.55237(15) 0.0506(13) Uani 1 1 d . . . . .
H1 H 0.4691 0.3006 0.5334 0.061 Uiso 1 1 calc R . . . .
C2 C 0.4768(5) 0.2621(5) 0.58476(18) 0.0612(15) Uani 1 1 d . . . . .
H2 H 0.5497 0.3117 0.5880 0.073 Uiso 1 1 calc R . . . .
C3 C 0.4181(5) 0.1962(5) 0.61246(17) 0.0637(16) Uani 1 1 d . . . . .
H3 H 0.4494 0.2015 0.6353 0.076 Uiso 1 1 calc R . . . .
C4 C 0.3120(5) 0.1217(5) 0.60649(15) 0.0581(14) Uani 1 1 d . . . . .
H4 H 0.2705 0.0736 0.6248 0.070 Uiso 1 1 calc R . . . .
C5 C 0.2691(4) 0.1195(4) 0.57364(14) 0.0463(12) Uani 1 1 d . . . . .
C6 C 0.1546(4) 0.0431(4) 0.56523(14) 0.0447(12) Uani 1 1 d . . . . .
H6A H 0.1348 -0.0275 0.5749 0.054 Uiso 1 1 calc R . . . .
H6B H 0.1096 0.0672 0.5769 0.054 Uiso 1 1 calc R . . . .
C7 C 0.3867(4) 0.3871(4) 0.46781(15) 0.0487(12) Uani 1 1 d . . . . .
H7 H 0.3618 0.4180 0.4848 0.058 Uiso 1 1 calc R . . . .
C8 C 0.4597(4) 0.4510(4) 0.44252(16) 0.0567(14) Uani 1 1 d . . . . .
H8 H 0.4841 0.5246 0.4419 0.068 Uiso 1 1 calc R . . . .
C9 C 0.4967(5) 0.4069(5) 0.41826(17) 0.0614(16) Uani 1 1 d . . . . .
H9 H 0.5474 0.4501 0.4008 0.074 Uiso 1 1 calc R . . . .
C10 C 0.4602(4) 0.2990(4) 0.41909(15) 0.0560(14) Uani 1 1 d . . . . .
H10 H 0.4853 0.2676 0.4024 0.067 Uiso 1 1 calc R . . . .
C11 C 0.3862(4) 0.2382(4) 0.44494(14) 0.0448(11) Uani 1 1 d . . . . .
C12 C 0.3431(4) 0.1205(4) 0.44819(15) 0.0501(13) Uani 1 1 d . . . . .
H12A H 0.3118 0.0859 0.4250 0.060 Uiso 1 1 calc R . . . .
H12B H 0.4014 0.1070 0.4539 0.060 Uiso 1 1 calc R . . . .
Cl1 Cl 0.6667 0.3333 0.48984(9) 0.0754(8) Uani 1 3 d S T P . .
O3 O 0.6667 0.3333 0.4510(3) 0.135(4) Uani 1 3 d S T P . .
O4 O 0.5924(4) 0.2282(4) 0.50044(18) 0.0971(18) Uani 1 1 d . . . . .
Cl2 Cl 0.0000 0.0000 0.65606(7) 0.0758(8) Uani 1 3 d S T P . .
O5 O 0.0000 0.0000 0.6930(2) 0.092(3) Uani 1 3 d S T P . .
O6 O 0.0686(6) 0.1045(5) 0.64347(17) 0.120(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.040(3) . ?
Ni1 O1 2.111(3) 12_556 ?
Ni1 O2 1.999(3) 12_556 ?
Ni1 O2 1.968(3) . ?
Ni1 N1 2.047(4) . ?
Ni1 N2 2.037(4) . ?
Ni2 O1 2.073(3) 11_556 ?
Ni2 O1 2.073(3) 12_556 ?
Ni2 O1 2.073(3) . ?
Ni2 O1 2.073(3) 3 ?
Ni2 O1 2.073(3) 10_556 ?
Ni2 O1 2.073(3) 2 ?
Cr1 O1 2.111(3) 12_556 ?
Cr1 O1 2.040(3) . ?
Cr1 O2 1.968(3) . ?
Cr1 O2 1.999(3) 12_556 ?
Cr1 N1 2.047(4) . ?
Cr1 N2 2.037(4) . ?
O1 Ni1 2.111(3) 11_556 ?
O1 Cr1 2.111(3) 11_556 ?
O1 C6 1.422(6) . ?
O2 Ni1 1.999(3) 11_556 ?
O2 Cr1 1.999(3) 11_556 ?
O2 C12 1.382(6) . ?
N1 C1 1.328(7) . ?
N1 C5 1.362(7) . ?
N2 C7 1.343(6) . ?
N2 C11 1.363(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.378(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(9) . ?
C3 H3 0.9500 . ?
C3 C4 1.397(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.369(8) . ?
C5 C6 1.508(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.380(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.369(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.389(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.388(7) . ?
C11 C12 1.512(7) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Cl1 O3 1.448(11) . ?
Cl1 O4 1.424(5) 3_665 ?
Cl1 O4 1.424(5) . ?
Cl1 O4 1.424(5) 2_655 ?
Cl2 O5 1.378(8) . ?
Cl2 O6 1.423(6) . ?
Cl2 O6 1.423(6) 2 ?
Cl2 O6 1.423(6) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 82.32(16) . 12_556 ?
O1 Ni1 N1 80.33(15) . . ?
O2 Ni1 O1 99.03(14) 12_556 . ?
O2 Ni1 O1 92.68(14) . 12_556 ?
O2 Ni1 O1 80.42(13) . . ?
O2 Ni1 O1 78.01(13) 12_556 12_556 ?
O2 Ni1 O2 170.64(13) . 12_556 ?
O2 Ni1 N1 91.54(15) 12_556 . ?
O2 Ni1 N1 97.56(15) . . ?
O2 Ni1 N2 81.46(15) . . ?
O2 Ni1 N2 98.96(16) 12_556 . ?
N1 Ni1 O1 158.05(15) . 12_556 ?
N2 Ni1 O1 161.87(14) . . ?
N2 Ni1 O1 99.28(14) . 12_556 ?
N2 Ni1 N1 101.40(17) . . ?
O1 Ni2 O1 180.0 10_556 . ?
O1 Ni2 O1 97.51(11) 10_556 11_556 ?
O1 Ni2 O1 82.49(11) 10_556 2 ?
O1 Ni2 O1 82.49(11) 11_556 . ?
O1 Ni2 O1 82.49(11) 11_556 3 ?
O1 Ni2 O1 82.49(11) 10_556 3 ?
O1 Ni2 O1 97.51(11) 2 . ?
O1 Ni2 O1 180.00(15) 11_556 2 ?
O1 Ni2 O1 97.51(11) 10_556 12_556 ?
O1 Ni2 O1 82.49(11) 12_556 . ?
O1 Ni2 O1 97.51(11) 3 . ?
O1 Ni2 O1 82.49(11) 2 12_556 ?
O1 Ni2 O1 97.51(11) 11_556 12_556 ?
O1 Ni2 O1 180.00(14) 12_556 3 ?
O1 Ni2 O1 97.51(11) 2 3 ?
O1 Cr1 O1 82.32(16) . 12_556 ?
O1 Cr1 N1 80.33(15) . . ?
O2 Cr1 O1 80.42(13) . . ?
O2 Cr1 O1 99.03(14) 12_556 . ?
O2 Cr1 O1 78.01(13) 12_556 12_556 ?
O2 Cr1 O1 92.68(14) . 12_556 ?
O2 Cr1 O2 170.64(13) . 12_556 ?
O2 Cr1 N1 91.54(15) 12_556 . ?
O2 Cr1 N1 97.56(15) . . ?
O2 Cr1 N2 98.96(16) 12_556 . ?
O2 Cr1 N2 81.46(15) . . ?
N1 Cr1 O1 158.05(15) . 12_556 ?
N2 Cr1 O1 161.87(14) . . ?
N2 Cr1 O1 99.28(14) . 12_556 ?
N2 Cr1 N1 101.40(17) . . ?
Ni1 O1 Ni1 97.62(13) . 11_556 ?
Ni1 O1 Ni2 98.67(13) . . ?
Ni2 O1 Ni1 96.42(13) . 11_556 ?
Ni2 O1 Cr1 96.42(13) . 11_556 ?
Cr1 O1 Ni2 98.67(13) . . ?
Cr1 O1 Cr1 97.62(13) . 11_556 ?
C6 O1 Ni1 111.2(3) . . ?
C6 O1 Ni1 118.7(3) . 11_556 ?
C6 O1 Ni2 128.6(3) . . ?
C6 O1 Cr1 118.7(3) . 11_556 ?
C6 O1 Cr1 111.2(3) . . ?
Ni1 O2 Ni1 103.93(15) . 11_556 ?
Cr1 O2 Cr1 103.93(15) . 11_556 ?
C12 O2 Ni1 118.0(3) . . ?
C12 O2 Ni1 137.9(3) . 11_556 ?
C12 O2 Cr1 118.0(3) . . ?
C12 O2 Cr1 137.9(3) . 11_556 ?
C1 N1 Ni1 128.0(4) . . ?
C1 N1 Cr1 128.0(4) . . ?
C1 N1 C5 118.8(5) . . ?
C5 N1 Ni1 113.1(3) . . ?
C5 N1 Cr1 113.1(3) . . ?
C7 N2 Ni1 127.7(4) . . ?
C7 N2 Cr1 127.7(4) . . ?
C7 N2 C11 119.2(4) . . ?
C11 N2 Ni1 113.1(3) . . ?
C11 N2 Cr1 113.1(3) . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.3(5) . . ?
C2 C1 H1 118.8 . . ?
C1 C2 H2 120.4 . . ?
C1 C2 C3 119.2(6) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(5) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.6(6) . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 122.1(5) . . ?
N1 C5 C6 116.0(4) . . ?
C4 C5 C6 121.9(5) . . ?
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 119.1 . . ?
N2 C7 C8 121.9(5) . . ?
C8 C7 H7 119.1 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.2(5) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.1(5) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.8 . . ?
C11 C10 C9 118.5(5) . . ?
C11 C10 H10 120.8 . . ?
N2 C11 C10 121.2(5) . . ?
N2 C11 C12 116.6(4) . . ?
C10 C11 C12 122.1(5) . . ?
O2 C12 C11 110.7(4) . . ?
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 106.1(3) 2_655 . ?
O4 Cl1 O3 106.1(3) 3_665 . ?
O4 Cl1 O3 106.1(3) . . ?
O4 Cl1 O4 112.6(3) 2_655 . ?
O4 Cl1 O4 112.6(3) 2_655 3_665 ?
O4 Cl1 O4 112.6(3) . 3_665 ?
O5 Cl2 O6 109.2(3) . 3 ?
O5 Cl2 O6 109.3(3) . 2 ?
O5 Cl2 O6 109.3(3) . . ?
O6 Cl2 O6 109.7(3) . 3 ?
O6 Cl2 O6 109.7(3) 2 3 ?
O6 Cl2 O6 109.7(3) 2 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C6 C5 -30.6(4) . . . . ?
Ni1 O1 C6 C5 81.3(4) 11_556 . . . ?
Ni1 O2 C12 C11 -2.8(6) . . . . ?
Ni1 O2 C12 C11 -178.3(3) 11_556 . . . ?
Ni1 N1 C1 C2 173.4(4) . . . . ?
Ni1 N1 C5 C4 -174.3(4) . . . . ?
Ni1 N1 C5 C6 4.9(5) . . . . ?
Ni1 N2 C7 C8 -177.1(4) . . . . ?
Ni1 N2 C11 C10 177.8(4) . . . . ?
Ni1 N2 C11 C12 -3.0(6) . . . . ?
Ni2 O1 C6 C5 -151.7(3) . . . . ?
Cr1 O1 C6 C5 81.3(4) 11_556 . . . ?
Cr1 O1 C6 C5 -30.6(4) . . . . ?
Cr1 O2 C12 C11 -2.8(6) . . . . ?
Cr1 O2 C12 C11 -178.3(3) 11_556 . . . ?
Cr1 N1 C1 C2 173.4(4) . . . . ?
Cr1 N1 C5 C4 -174.3(4) . . . . ?
Cr1 N1 C5 C6 4.9(5) . . . . ?
Cr1 N2 C7 C8 -177.1(4) . . . . ?
Cr1 N2 C11 C10 177.8(4) . . . . ?
Cr1 N2 C11 C12 -3.0(6) . . . . ?
N1 C1 C2 C3 0.1(9) . . . . ?
N1 C5 C6 O1 17.2(6) . . . . ?
N2 C7 C8 C9 -0.8(8) . . . . ?
N2 C11 C12 O2 3.8(7) . . . . ?
C1 N1 C5 C4 1.8(8) . . . . ?
C1 N1 C5 C6 -179.0(4) . . . . ?
C1 C2 C3 C4 2.2(9) . . . . ?
C2 C3 C4 C5 -2.4(9) . . . . ?
C3 C4 C5 N1 0.4(8) . . . . ?
C3 C4 C5 C6 -178.7(5) . . . . ?
C4 C5 C6 O1 -163.7(5) . . . . ?
C5 N1 C1 C2 -2.1(8) . . . . ?
C7 N2 C11 C10 -0.3(7) . . . . ?
C7 N2 C11 C12 178.9(5) . . . . ?
C7 C8 C9 C10 0.5(9) . . . . ?
C8 C9 C10 C11 -0.1(9) . . . . ?
C9 C10 C11 N2 0.0(8) . . . . ?
C9 C10 C11 C12 -179.1(5) . . . . ?
C10 C11 C12 O2 -177.0(5) . . . . ?
C11 N2 C7 C8 0.7(7) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-11
_olex2_date_sample_submission    2016-04-11
_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 527o
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_CHEMW03_1                   
;
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_4
_database_code_depnum_ccdc_archive 'CCDC 1819134'
_audit_update_record             
;
2018-01-24 deposited with the CCDC.
2018-03-15 downloaded from the CCDC.
;
# local name eb17005
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H72 Al2 N12 O12 Zn5, 4(Cl1 O4), 8 C H4 O'
_chemical_formula_sum            'C80 H104 Al2 Cl4 N12 O36 Zn5'
_chemical_formula_weight         2332.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Zn Cl Al'
_chemical_oxdiff_usercomment     '@ 120 K 805o'
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'
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'
Zn Zn 0.2839 1.4301 '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                   14.4962(5)
_cell_length_b                   14.4962(5)
_cell_length_c                   38.022(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6919.4(6)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    3072
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      26.3140
_cell_measurement_theta_min      3.2870
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_correction_T_min  0.7260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0706 before and 0.0552 after correction. The Ratio of minimum to maximum transmission is 0.7319. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3600
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 18 -7 0.1181
0 0 -1 0.0199
17 1 -3 0.1133
18 -17 4 0.1123
-3 -16 7 0.1121
-18 1 2 0.1066
-17 18 -5 0.1232
0 0 1 0.0199

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.04
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
-0.4253 17.7460 -7.3038 0.0861 -0.4699 0.8785
0.0000 0.0001 -0.9944 0.0182 0.0025 0.0024
17.0214 1.2447 -2.8954 0.1824 -0.9810 0.0669
18.3504 -16.8177 4.4134 0.1040 -0.5525 -0.8270
-2.7114 -16.0371 7.0331 -0.1098 0.5968 -0.7949
-18.1022 0.8619 2.1724 -0.1828 0.9825 0.0371
-17.4837 17.7520 -4.9222 -0.0903 0.4783 0.8735
-0.0000 -0.0001 0.9944 -0.0182 -0.0025 -0.0024

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            13554
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.810
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  13.00   1.00   30.00    --   -9.43  38.00 -90.00   27
  2  ω    -62.00  38.00   1.00   30.00    --   10.92 -77.00-120.00  100
  3  ω      7.00  39.00   1.00   30.00    --   10.92  57.00 150.00   32
  4  ω    -37.00   5.00   1.00   30.00    --   10.92 -38.00 -30.00   42
  5  ω    -27.00   1.00   1.00   30.00    --   10.92 -38.00  30.00   28
;
_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      0.0077818000
_diffrn_orient_matrix_UB_12      -0.0025007000
_diffrn_orient_matrix_UB_13      -0.0183138000
_diffrn_orient_matrix_UB_21      -0.0559547000
_diffrn_orient_matrix_UB_22      -0.0288740000
_diffrn_orient_matrix_UB_23      -0.0025618000
_diffrn_orient_matrix_UB_31      -0.0000322000
_diffrn_orient_matrix_UB_32      0.0484959000
_diffrn_orient_matrix_UB_33      -0.0024501000
_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                2492
_reflns_number_total             3142
_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 1.171.38.43 (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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3142
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0647
_refine_ls_restrained_S_all      1.091
_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)+(0.0403P)²+65.7332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1459
_refine_special_details          
;
Merohedral twinning was handled with twin law [0 -1 0 / -1 0 0 / 0 0 -1] and refined twin scale factor 0.256(2).  The SQUEEZE routine of PLATON was used to account for electron density which corresponds to eight molecules of methanol per complete wheel.  This missing solvent is included in the total chemical formula, triggering a lot of checkCIF alerts, which should be ignored.  Zn1 and Al1 were modelled with occupancies fixed such that the ratio 5:2 is observed in the wheel.  This is consistent with free refinement of occupancies, and with charge balance considerations.

#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0095 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      7.023 Check
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.259 Check

Not significant

#===============================================================================
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.1843 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      65.73 Why ?

See above for a discussion of twinning and squeeze.

171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records          1 Report
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl1 Check
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
300_ALERT_4_G Atom Site Occupancy of >Zn1    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
605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        459 A**3
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
870_ALERT_4_G ALERTS Related to Twinning Effects Suppressed ..          ! Info
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           4 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note

Nothing here is significant or relates to something other than twinning or squeeze.

#===============================================================================
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.744(2) 0.256(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Shared sites
{Zn1, Al1}
4. Uiso/Uaniso restraints and constraints
Uanis(Zn1) = Uanis(Al1)
5. Others
 Fixed Sof: Zn1(0.66666) Al1(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
6.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
Zn1 Zn 0.60193(6) 0.51319(6) 0.33741(2) 0.0238(2) Uani 0.6667 1 d . . . A 1
Al1 Al 0.60193(6) 0.51319(6) 0.33741(2) 0.0238(2) Uani 0.3333 1 d . . . A 2
Zn2 Zn 0.666667 0.333333 0.333333 0.0215(3) Uani 1 6 d S T P A .
Cl1 Cl 1.000000 1.000000 0.33823(10) 0.0597(9) Uani 1 3 d S T P . .
O1 O 0.5632(3) 0.3690(3) 0.36059(8) 0.0239(7) Uani 1 1 d . . . . .
O2 O 0.4737(3) 0.4114(3) 0.31097(9) 0.0265(8) Uani 1 1 d . . . . .
O3 O 0.8956(4) 0.9260(4) 0.33225(18) 0.0780(18) Uani 1 1 d . . . . .
O4 O 1.000000 1.000000 0.3796(3) 0.137(5) Uani 1 3 d S T P . .
N1 N 0.5271(3) 0.5212(3) 0.38187(12) 0.0285(10) Uani 1 1 d . . . . .
N2 N 0.5935(3) 0.6147(3) 0.30242(11) 0.0259(9) Uani 1 1 d . . . . .
C1 C 0.4956(4) 0.5901(4) 0.38878(19) 0.0415(15) Uani 1 1 d . . . . .
H1 H 0.501242 0.638275 0.370834 0.050 Uiso 1 1 calc R . . . .
C2 C 0.4546(5) 0.5953(5) 0.4210(2) 0.0534(18) Uani 1 1 d . . . . .
H2 H 0.433298 0.646561 0.425206 0.064 Uiso 1 1 calc R . . . .
C3 C 0.4453(5) 0.5251(5) 0.4468(2) 0.0534(18) Uani 1 1 d . . . . .
H3 H 0.418322 0.527999 0.469335 0.064 Uiso 1 1 calc R . . . .
C4 C 0.4753(5) 0.4503(5) 0.43994(16) 0.0406(14) Uani 1 1 d . . . . .
H4 H 0.468474 0.400145 0.457327 0.049 Uiso 1 1 calc R . . . .
C5 C 0.5156(4) 0.4505(4) 0.40692(14) 0.0287(12) Uani 1 1 d . . . . .
C6 C 0.5508(4) 0.3711(4) 0.39743(13) 0.0281(11) Uani 1 1 d . . . . .
H6A H 0.619214 0.391255 0.409223 0.034 Uiso 1 1 calc R . . . .
H6B H 0.497051 0.299273 0.405746 0.034 Uiso 1 1 calc R . . . .
C7 C 0.6627(5) 0.7201(4) 0.29939(17) 0.0407(15) Uani 1 1 d . . . . .
H7 H 0.719576 0.752979 0.315776 0.049 Uiso 1 1 calc R . . . .
C8 C 0.6543(6) 0.7808(5) 0.2740(2) 0.0529(19) Uani 1 1 d . . . . .
H8 H 0.704864 0.854619 0.272414 0.063 Uiso 1 1 calc R . . . .
C9 C 0.5709(7) 0.7333(6) 0.2505(2) 0.060(2) Uani 1 1 d . . . . .
H9 H 0.563160 0.774289 0.232406 0.072 Uiso 1 1 calc R . . . .
C10 C 0.5006(5) 0.6285(5) 0.25333(17) 0.0460(16) Uani 1 1 d . . . . .
H10 H 0.442537 0.594982 0.237408 0.055 Uiso 1 1 calc R . . . .
C11 C 0.5134(4) 0.5699(4) 0.27961(14) 0.0299(12) Uani 1 1 d . . . . .
C12 C 0.4381(4) 0.4515(4) 0.28399(15) 0.0342(13) Uani 1 1 d . . . . .
H12A H 0.365868 0.438377 0.289622 0.041 Uiso 1 1 calc R . . . .
H12B H 0.434092 0.414372 0.261699 0.041 Uiso 1 1 calc R . . . .
Cl2 Cl 0.333333 0.666667 0.51173(7) 0.0543(7) Uani 1 3 d S T P . .
O5 O 0.333333 0.666667 0.4749(2) 0.070(3) Uani 1 3 d S T P . .
O6 O 0.2992(6) 0.5635(5) 0.52479(17) 0.101(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.071(3) . ?
Zn1 O1 2.179(3) 17 ?
Zn1 O2 1.975(3) . ?
Zn1 O2 1.944(3) 17 ?
Zn1 N1 2.043(4) . ?
Zn1 N2 2.032(4) . ?
Al1 O1 2.179(3) 17 ?
Al1 O1 2.071(3) . ?
Al1 O2 1.944(3) 17 ?
Al1 O2 1.975(3) . ?
Al1 N1 2.043(4) . ?
Al1 N2 2.032(4) . ?
Zn2 O1 2.089(3) 17 ?
Zn2 O1 2.089(3) 18_545 ?
Zn2 O1 2.089(3) 2_655 ?
Zn2 O1 2.089(3) . ?
Zn2 O1 2.089(3) 3_665 ?
Zn2 O1 2.089(3) 16_655 ?
Cl1 O3 1.367(5) . ?
Cl1 O3 1.367(5) 3_675 ?
Cl1 O3 1.367(5) 2_765 ?
Cl1 O4 1.572(13) . ?
O1 C6 1.414(6) . ?
O2 C12 1.398(6) . ?
N1 C1 1.317(7) . ?
N1 C5 1.347(7) . ?
N2 C7 1.350(7) . ?
N2 C11 1.329(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.380(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.371(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.382(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(8) . ?
C5 C6 1.518(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.351(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.381(11) . ?
C9 H9 0.9500 . ?
C9 C10 1.345(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(8) . ?
C11 C12 1.514(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Cl2 O5 1.401(9) . ?
Cl2 O6 1.411(6) 2_665 ?
Cl2 O6 1.411(6) 3_565 ?
Cl2 O6 1.411(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 80.77(17) . 17 ?
O2 Zn1 O1 101.14(14) 17 . ?
O2 Zn1 O1 77.52(13) . . ?
O2 Zn1 O1 75.61(13) 17 17 ?
O2 Zn1 O1 91.50(14) . 17 ?
O2 Zn1 O2 167.05(14) 17 . ?
O2 Zn1 N1 97.79(16) . . ?
O2 Zn1 N1 94.61(15) 17 . ?
O2 Zn1 N2 80.36(16) . . ?
O2 Zn1 N2 99.85(16) 17 . ?
N1 Zn1 O1 79.72(15) . . ?
N1 Zn1 O1 155.99(15) . 17 ?
N2 Zn1 O1 97.39(14) . 17 ?
N2 Zn1 O1 157.73(15) . . ?
N2 Zn1 N1 105.95(17) . . ?
O1 Al1 O1 80.77(17) . 17 ?
O2 Al1 O1 75.61(13) 17 17 ?
O2 Al1 O1 101.14(14) 17 . ?
O2 Al1 O1 77.52(13) . . ?
O2 Al1 O1 91.50(14) . 17 ?
O2 Al1 O2 167.05(14) 17 . ?
O2 Al1 N1 97.79(16) . . ?
O2 Al1 N1 94.61(15) 17 . ?
O2 Al1 N2 80.36(16) . . ?
O2 Al1 N2 99.85(16) 17 . ?
N1 Al1 O1 155.99(15) . 17 ?
N1 Al1 O1 79.72(15) . . ?
N2 Al1 O1 97.39(14) . 17 ?
N2 Al1 O1 157.73(15) . . ?
N2 Al1 N1 105.95(17) . . ?
O1 Zn2 O1 180.00(11) 16_655 . ?
O1 Zn2 O1 97.52(11) 2_655 . ?
O1 Zn2 O1 82.47(11) 16_655 2_655 ?
O1 Zn2 O1 82.48(11) 17 . ?
O1 Zn2 O1 97.53(11) 3_665 . ?
O1 Zn2 O1 180.0 18_545 3_665 ?
O1 Zn2 O1 97.52(11) 16_655 18_545 ?
O1 Zn2 O1 82.47(11) 18_545 2_655 ?
O1 Zn2 O1 82.48(11) 17 3_665 ?
O1 Zn2 O1 97.52(11) 16_655 17 ?
O1 Zn2 O1 82.48(11) 16_655 3_665 ?
O1 Zn2 O1 97.52(11) 18_545 17 ?
O1 Zn2 O1 180.0 17 2_655 ?
O1 Zn2 O1 82.48(11) 18_545 . ?
O1 Zn2 O1 97.53(11) 2_655 3_665 ?
O3 Cl1 O3 117.29(19) . 3_675 ?
O3 Cl1 O3 117.29(19) . 2_765 ?
O3 Cl1 O3 117.29(19) 3_675 2_765 ?
O3 Cl1 O4 99.6(3) 3_675 . ?
O3 Cl1 O4 99.6(3) 2_765 . ?
O3 Cl1 O4 99.6(3) . . ?
Zn1 O1 Zn1 97.56(13) . 18_545 ?
Zn1 O1 Zn2 99.96(14) . . ?
Al1 O1 Zn2 99.96(14) . . ?
Zn2 O1 Zn1 96.54(13) . 18_545 ?
C6 O1 Zn1 118.0(3) . 18_545 ?
C6 O1 Zn1 111.9(3) . . ?
C6 O1 Al1 111.9(3) . . ?
C6 O1 Zn2 127.7(3) . . ?
Zn1 O2 Zn1 109.30(16) 18_545 . ?
C12 O2 Zn1 117.9(3) . . ?
C12 O2 Zn1 132.8(3) . 18_545 ?
C12 O2 Al1 117.9(3) . . ?
C1 N1 Zn1 127.2(4) . . ?
C1 N1 Al1 127.2(4) . . ?
C1 N1 C5 118.6(5) . . ?
C5 N1 Zn1 114.2(3) . . ?
C5 N1 Al1 114.2(3) . . ?
C7 N2 Zn1 126.6(4) . . ?
C7 N2 Al1 126.6(4) . . ?
C11 N2 Zn1 115.3(3) . . ?
C11 N2 Al1 115.3(3) . . ?
C11 N2 C7 118.0(5) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.8(6) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.8(6) . . ?
C3 C2 H2 120.6 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.6(6) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 121.0 . . ?
C3 C4 C5 117.9(6) . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 122.4(5) . . ?
N1 C5 C6 116.6(4) . . ?
C4 C5 C6 121.0(5) . . ?
O1 C6 C5 110.3(4) . . ?
O1 C6 H6A 109.6 . . ?
O1 C6 H6B 109.6 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
N2 C7 H7 118.7 . . ?
N2 C7 C8 122.7(7) . . ?
C8 C7 H7 118.7 . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.7(6) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.3(6) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 120.2 . . ?
C9 C10 C11 119.6(7) . . ?
C11 C10 H10 120.2 . . ?
N2 C11 C10 121.6(5) . . ?
N2 C11 C12 116.1(4) . . ?
C10 C11 C12 122.3(5) . . ?
O2 C12 C11 110.2(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 . . ?
O5 Cl2 O6 110.6(3) . 3_565 ?
O5 Cl2 O6 110.6(3) . . ?
O5 Cl2 O6 110.6(3) . 2_665 ?
O6 Cl2 O6 108.3(3) 3_565 . ?
O6 Cl2 O6 108.3(3) 3_565 2_665 ?
O6 Cl2 O6 108.3(3) 2_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
Zn1 O1 C6 C5 27.9(5) . . . . ?
Zn1 O1 C6 C5 -84.1(4) 18_545 . . . ?
Zn1 O2 C12 C11 -176.6(3) 18_545 . . . ?
Zn1 O2 C12 C11 3.0(6) . . . . ?
Zn1 N1 C1 C2 -173.7(5) . . . . ?
Zn1 N1 C5 C4 174.2(4) . . . . ?
Zn1 N1 C5 C6 -4.9(6) . . . . ?
Zn1 N2 C7 C8 176.2(4) . . . . ?
Zn1 N2 C11 C10 -177.1(4) . . . . ?
Zn1 N2 C11 C12 2.5(6) . . . . ?
Al1 O1 C6 C5 27.9(5) . . . . ?
Al1 O2 C12 C11 3.0(6) . . . . ?
Al1 N1 C1 C2 -173.7(5) . . . . ?
Al1 N1 C5 C4 174.2(4) . . . . ?
Al1 N1 C5 C6 -4.9(6) . . . . ?
Al1 N2 C7 C8 176.2(4) . . . . ?
Al1 N2 C11 C10 -177.1(4) . . . . ?
Al1 N2 C11 C12 2.5(6) . . . . ?
Zn2 O1 C6 C5 150.9(3) . . . . ?
N1 C1 C2 C3 -0.7(10) . . . . ?
N1 C5 C6 O1 -15.5(6) . . . . ?
N2 C7 C8 C9 0.8(9) . . . . ?
N2 C11 C12 O2 -3.5(7) . . . . ?
C1 N1 C5 C4 -2.2(8) . . . . ?
C1 N1 C5 C6 178.7(5) . . . . ?
C1 C2 C3 C4 -1.0(10) . . . . ?
C2 C3 C4 C5 1.0(10) . . . . ?
C3 C4 C5 N1 0.6(9) . . . . ?
C3 C4 C5 C6 179.7(5) . . . . ?
C4 C5 C6 O1 165.3(5) . . . . ?
C5 N1 C1 C2 2.3(8) . . . . ?
C7 N2 C11 C10 0.2(8) . . . . ?
C7 N2 C11 C12 179.8(5) . . . . ?
C7 C8 C9 C10 -0.1(10) . . . . ?
C8 C9 C10 C11 -0.5(10) . . . . ?
C9 C10 C11 N2 0.4(9) . . . . ?
C9 C10 C11 C12 -179.2(6) . . . . ?
C10 C11 C12 O2 176.1(5) . . . . ?
C11 N2 C7 C8 -0.8(8) . . . . ?

_olex2_date_sample_data_collection 2017-01-13
_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 805o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.884
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.744(2)
2 0.256(2)

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1819133'
_audit_update_record             
;
2018-01-24 deposited with the CCDC.
2018-03-15 downloaded from the CCDC.
;
# local name eb16257
_audit_creation_date             2016-11-15
_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 N12 Ni5 O12, 4(Cl1 O4), 9 C H4 O'
_chemical_formula_sum            'C81 H108 Al2 Cl4 N12 Ni5 O37'
_chemical_formula_weight         2331.10
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Ni Cl Al'
_chemical_oxdiff_usercomment     '@ 120 K 754o SOC'
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'
Al Al 0.2130 0.2455 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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                   14.53160(10)
_cell_length_b                   14.53160(10)
_cell_length_c                   37.9260(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6935.77(19)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    20349
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      75.3420
_cell_measurement_theta_min      4.1950
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.195
_exptl_absorpt_correction_T_max  0.9480
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0943 before and 0.0760 after correction.
The Ratio of minimum to maximum transmission is 0.6782.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3624
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 -9 5 0.1044
-3 9 -4 0.0720
9 -4 4 0.1173
2 7 -1 0.0976
-8 0 -2 0.0904
-2 -7 1 0.0964
1 -1 -24 0.0115
8 0 -7 0.1102
-3 1 24 0.0515
5 0 19 0.1217

_exptl_crystal_recrystallization_method 
'The material was recrystallised from methanol by hydrothermal bomb'
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.089
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
6.9938 -8.9906 5.0152 0.2771 -0.9236 -0.3368
-2.9978 8.9927 -4.0182 -0.2874 0.9288 -0.1540
8.9912 -3.9928 4.0022 0.1203 -0.4014 -0.8735
1.9969 6.9966 -1.0180 -0.1934 0.7327 -0.6557
-7.9920 -0.0041 -1.9940 0.0206 -0.0104 0.9816
-1.9969 -6.9966 1.0180 0.1934 -0.7327 0.6557
1.0094 -1.0014 -23.9840 -0.9575 -0.2157 0.0367
7.9958 0.0032 -7.0007 -0.3818 -0.0311 -0.9445
-3.0076 1.0004 23.9852 0.9827 0.2154 0.2066
4.9875 0.0044 18.9858 0.6995 0.0883 -0.6866

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            32013
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.591
_diffrn_reflns_theta_min         3.700
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  29.00   1.00   10.00    --  -43.17  38.00 -90.00   95
  2  ω    -70.00  27.00   1.00   10.00    --  -43.17  57.00  90.00   97
  3  ω   -100.00  -7.00   1.00   10.00    --  -43.17 133.00 -49.00   93
  4  ω    -66.00  29.00   1.00   10.00    --  -43.17  38.00-180.00   95
  5  ω   -113.00 -17.00   1.00   10.00    --  -43.17 -57.00 -60.00   96
  6  ω     23.00  98.00   1.00   10.00    --   43.17-125.00-120.00   75
  7  ω     41.00 128.00   1.00   30.00    --  111.00-137.00  64.00   87
  8  ω     83.00 178.00   1.00   30.00    --  111.00  61.00 -30.00   95
  9  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00  60.00   79
 10  ω     94.00 178.00   1.00   30.00    --  111.00 125.00-180.00   84
 11  ω     37.00 142.00   1.00   30.00    --  111.00 -77.00 -60.00  105
 12  ω     39.00 121.00   1.00   30.00    --  111.00-125.00 -30.00   82
 13  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00  90.00   79
 14  ω     83.00 178.00   1.00   30.00    --  111.00  61.00-180.00   95
 15  ω     30.00 109.00   1.00   30.00    --  111.00 -94.00 150.00   79
 16  ω     41.00 139.00   1.00   30.00    --  111.00 -61.00-180.00   98
 17  ω     39.00 121.00   1.00   30.00    --  111.00-125.00  30.00   82
 18  ω     39.00 121.00   1.00   30.00    --  111.00-125.00 -90.00   82
 19  ω     39.00 121.00   1.00   30.00    --  111.00-125.00 150.00   82
 20  ω     87.00 161.00   1.00   30.00    --  111.00  45.00 -60.00   74
 21  ω     72.00 125.00   1.00   30.00    --  111.00-133.00-117.00   53
 22  ω    109.00 153.00   1.00   30.00    --  111.00  61.00-120.00   44
 23  ω     81.00 106.00   1.00   30.00    --  111.00  77.00-120.00   25
 24  ω    118.00 176.00   1.00   30.00    --  111.00  77.00-120.00   58
 25  ω     67.00 108.00   1.00   30.00    --  111.00 -94.00  30.00   41
 26  ω     55.00  85.00   1.00   30.00    --  111.00 -94.00 120.00   30
 27  ω    133.00 159.00   1.00   30.00    --  111.00 125.00 -90.00   26
 28  ω     55.00  81.00   1.00   30.00    --  111.00-125.00  60.00   26
 29  ω    112.00 156.00   1.00   30.00    --  111.00 -15.00  60.00   44
 30  ω     34.00  96.00   1.00   30.00    --  111.00 -15.00  60.00   62
;
_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      -0.0125820000
_diffrn_orient_matrix_UB_12      -0.0182141000
_diffrn_orient_matrix_UB_13      0.0401524000
_diffrn_orient_matrix_UB_21      0.0000989000
_diffrn_orient_matrix_UB_22      0.1053696000
_diffrn_orient_matrix_UB_23      0.0046000000
_diffrn_orient_matrix_UB_31      -0.1217544000
_diffrn_orient_matrix_UB_32      -0.0595794000
_diffrn_orient_matrix_UB_33      -0.0041674000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3044
_reflns_number_total             3217
_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         0.878
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0818
_refine_ls_restrained_S_all      1.134
_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)+(0.1395P)²+42.4831P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2373
_refine_ls_wR_factor_ref         0.2395
_refine_special_details          
;
The SQUEEZE routine of PLATON was used to handle electron density approximating to 27 molecule of methanol per unit cell, or 9 molecules per complete wheel.  This missing solvent is included in the total chemical 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
 
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0082 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      4.544 Check
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          2 Report

Not serious

#===============================================================================
041_ALERT_1_G Calc. and Reported SumFormula    Strings  Differ     Please Check
044_ALERT_1_G Calculated and Reported Density Dx  Differ by ..     0.2069 Check
051_ALERT_1_G Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       4.82 %
068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check
072_ALERT_2_G SHELXL First  Parameter in WGHT  Unusually Large       0.14 Report
083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      42.48 Why ?

All a consequence of SQUEEZE

171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records          1 Report
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni1    --  O1      ..        6.3 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Ni1    --  N2      ..        5.3 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Al1    --  O1      ..        6.3 s.u.
232_ALERT_2_G Hirshfeld Test Diff (M-X)  Al1    --  N2      ..        5.3 s.u.

Disordered mix of Al and Ni, necessary for charge balance and supported by other analytical data

244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl1 Check
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
300_ALERT_4_G Atom Site Occupancy of >Ni1    is Constrained at     0.6667 Check
300_ALERT_4_G Atom Site Occupancy of <Al1    is Constrained at     0.3333 Check

Nothing serious

301_ALERT_3_G Main Residue  Disorder ............ Percentage =          4 Note

Substitutional disorder

605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        472 A**3
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info

Consequence of SQUEEZE, discussed above

910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           1 Note
912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         40 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Ni1, Al1}
3. Uiso/Uaniso restraints and constraints
Uanis(Ni1) = Uanis(Al1)
4. Others
 Fixed Sof: Ni1(0.66667) Al1(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(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
Ni1 Ni 0.50701(6) 0.60324(6) 0.66390(2) 0.0311(3) Uani 0.6667 1 d . . . A 2
Al1 Al 0.50701(6) 0.60324(6) 0.66390(2) 0.0311(3) Uani 0.3333 1 d . . . A 2
Ni2 Ni 0.333333 0.666667 0.666667 0.0299(4) Uani 1 6 d S T P A .
O1 O 0.3690(2) 0.5653(2) 0.63984(8) 0.0353(6) Uani 1 1 d . . . . .
O2 O 0.4092(2) 0.4776(2) 0.69021(8) 0.0393(6) Uani 1 1 d . . . . .
N1 N 0.5217(3) 0.5277(3) 0.62113(11) 0.0442(8) Uani 1 1 d . . . . .
N2 N 0.6127(3) 0.5974(3) 0.69770(9) 0.0363(7) Uani 1 1 d . . . . .
C1 C 0.5889(4) 0.4937(4) 0.61488(14) 0.0501(11) Uani 1 1 d . . . . .
H1 H 0.634020 0.497194 0.633574 0.060 Uiso 1 1 calc R . . . .
C2 C 0.5979(4) 0.4537(4) 0.58318(17) 0.0594(13) Uani 1 1 d . . . . .
H2 H 0.649230 0.432135 0.579927 0.071 Uiso 1 1 calc R . . . .
C3 C 0.5299(5) 0.4452(5) 0.55571(17) 0.0646(14) Uani 1 1 d . . . . .
H3 H 0.534543 0.418364 0.533352 0.078 Uiso 1 1 calc R . . . .
C4 C 0.4548(4) 0.4770(4) 0.56169(14) 0.0558(12) Uani 1 1 d . . . . .
H4 H 0.406485 0.470605 0.543703 0.067 Uiso 1 1 calc R . . . .
C5 C 0.4527(4) 0.5177(3) 0.59424(13) 0.0452(10) Uani 1 1 d . . . . .
C6 C 0.3749(4) 0.5558(4) 0.60272(12) 0.0449(10) Uani 1 1 d . . . . .
H6A H 0.398633 0.625452 0.591389 0.054 Uiso 1 1 calc R . . . .
H6B H 0.303706 0.504512 0.593356 0.054 Uiso 1 1 calc R . . . .
C7 C 0.7176(3) 0.6653(3) 0.69922(12) 0.0412(9) Uani 1 1 d . . . . .
H7 H 0.748776 0.721730 0.682634 0.049 Uiso 1 1 calc R . . . .
C8 C 0.7821(4) 0.6559(4) 0.72415(15) 0.0532(12) Uani 1 1 d . . . . .
H8 H 0.856294 0.704940 0.724595 0.064 Uiso 1 1 calc R . . . .
C9 C 0.7369(4) 0.5746(5) 0.74822(15) 0.0576(13) Uani 1 1 d . . . . .
H9 H 0.779385 0.566798 0.765699 0.069 Uiso 1 1 calc R . . . .
C10 C 0.6283(4) 0.5038(4) 0.74663(13) 0.0507(11) Uani 1 1 d . . . . .
H10 H 0.595512 0.446897 0.763019 0.061 Uiso 1 1 calc R . . . .
C11 C 0.5684(3) 0.5171(3) 0.72089(11) 0.0400(9) Uani 1 1 d . . . . .
C12 C 0.4504(3) 0.4434(3) 0.71694(12) 0.0418(9) Uani 1 1 d . . . . .
H12A H 0.436394 0.370873 0.711506 0.050 Uiso 1 1 calc R . . . .
H12B H 0.414520 0.440446 0.739440 0.050 Uiso 1 1 calc R . . . .
Cl1 Cl 0.666667 0.333333 0.67598(9) 0.0791(8) Uani 1 3 d S T P . .
O3 O 0.5615(4) 0.3021(4) 0.66643(19) 0.0993(19) Uani 1 1 d . . . . .
O4 O 0.666667 0.333333 0.7143(3) 0.138(5) Uani 1 3 d S T P . .
Cl2 Cl 0.333333 0.666667 0.51041(8) 0.0957(10) Uani 1 3 d S T P . .
O5 O 0.333333 0.666667 0.4738(2) 0.090(3) Uani 1 3 d S T P . .
O6 O 0.4336(8) 0.6914(10) 0.5236(2) 0.174(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.013(3) . ?
Ni1 O1 2.094(3) 15_556 ?
Ni1 O2 1.948(3) 15_556 ?
Ni1 O2 1.938(3) . ?
Ni1 N1 2.029(4) . ?
Ni1 N2 2.035(4) . ?
Ni2 O1 2.059(3) 14_456 ?
Ni2 O1 2.059(3) 3_565 ?
Ni2 O1 2.059(3) 13_566 ?
Ni2 O1 2.059(3) . ?
Ni2 O1 2.059(3) 15_556 ?
Ni2 O1 2.059(3) 2_665 ?
O1 C6 1.421(6) . ?
O2 C12 1.389(5) . ?
N1 C1 1.317(6) . ?
N1 C5 1.386(6) . ?
N2 C7 1.340(5) . ?
N2 C11 1.341(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.370(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.399(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.399(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.376(7) . ?
C5 C6 1.521(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.385(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.373(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.389(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(6) . ?
C11 C12 1.508(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Cl1 O3 1.407(5) 2_655 ?
Cl1 O3 1.407(6) 3_665 ?
Cl1 O3 1.407(5) . ?
Cl1 O4 1.454(12) . ?
Cl2 O5 1.388(8) . ?
Cl2 O6 1.407(8) 2_665 ?
Cl2 O6 1.407(8) 3_565 ?
Cl2 O6 1.407(8) . ?

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 Ni1 O1 82.56(15) . 15_556 ?
O1 Ni1 N1 81.34(14) . . ?
O1 Ni1 N2 160.65(13) . . ?
O2 Ni1 O1 93.06(13) . 15_556 ?
O2 Ni1 O1 77.13(12) 15_556 15_556 ?
O2 Ni1 O1 99.74(12) 15_556 . ?
O2 Ni1 O1 79.31(12) . . ?
O2 Ni1 O2 170.17(12) . 15_556 ?
O2 Ni1 N1 97.36(14) . . ?
O2 Ni1 N1 92.15(13) 15_556 . ?
O2 Ni1 N2 81.33(13) . . ?
O2 Ni1 N2 99.33(14) 15_556 . ?
N1 Ni1 O1 158.83(15) . 15_556 ?
N1 Ni1 N2 101.24(15) . . ?
N2 Ni1 O1 98.51(13) . 15_556 ?
O1 Ni2 O1 97.68(11) 13_566 14_456 ?
O1 Ni2 O1 180.0 15_556 3_565 ?
O1 Ni2 O1 82.32(11) 13_566 3_565 ?
O1 Ni2 O1 82.32(11) 14_456 . ?
O1 Ni2 O1 97.68(11) 3_565 . ?
O1 Ni2 O1 180.0 14_456 2_665 ?
O1 Ni2 O1 97.68(11) 3_565 2_665 ?
O1 Ni2 O1 82.32(11) 14_456 3_565 ?
O1 Ni2 O1 82.32(11) 15_556 2_665 ?
O1 Ni2 O1 97.68(11) 14_456 15_556 ?
O1 Ni2 O1 180.0 13_566 . ?
O1 Ni2 O1 82.32(11) 13_566 2_665 ?
O1 Ni2 O1 82.32(11) 15_556 . ?
O1 Ni2 O1 97.68(11) 13_566 15_556 ?
O1 Ni2 O1 97.68(11) 2_665 . ?
Ni1 O1 Ni2 98.79(12) . . ?
Ni2 O1 Ni1 96.23(12) . 14_456 ?
C6 O1 Ni1 112.1(2) . . ?
C6 O1 Ni1 119.1(2) . 14_456 ?
C6 O1 Ni2 127.4(2) . . ?
C12 O2 Ni1 118.0(2) . . ?
C12 O2 Ni1 136.4(3) . 14_456 ?
C1 N1 Ni1 130.2(4) . . ?
C1 N1 C5 117.5(4) . . ?
C5 N1 Ni1 112.2(3) . . ?
C7 N2 Ni1 126.9(3) . . ?
C7 N2 C11 119.1(4) . . ?
C11 N2 Ni1 113.9(3) . . ?
N1 C1 H1 117.8 . . ?
N1 C1 C2 124.3(5) . . ?
C2 C1 H1 117.8 . . ?
C1 C2 H2 120.8 . . ?
C1 C2 C3 118.5(5) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 118.9(5) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.5(5) . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C6 115.9(4) . . ?
C4 C5 N1 122.3(4) . . ?
C4 C5 C6 121.8(4) . . ?
O1 C6 C5 109.7(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 118.9 . . ?
N2 C7 C8 122.2(4) . . ?
C8 C7 H7 118.9 . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.9(4) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 120.5 . . ?
C8 C9 C10 119.1(5) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.2(5) . . ?
C11 C10 H10 120.4 . . ?
N2 C11 C10 121.5(4) . . ?
N2 C11 C12 115.7(3) . . ?
C10 C11 C12 122.8(4) . . ?
O2 C12 C11 111.0(3) . . ?
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 113.6(3) 2_655 3_665 ?
O3 Cl1 O3 113.6(3) 2_655 . ?
O3 Cl1 O3 113.6(3) 3_665 . ?
O3 Cl1 O4 104.9(3) 2_655 . ?
O3 Cl1 O4 104.9(3) 3_665 . ?
O3 Cl1 O4 104.9(3) . . ?
O5 Cl2 O6 110.8(4) . 2_665 ?
O5 Cl2 O6 110.8(4) . 3_565 ?
O5 Cl2 O6 110.8(4) . . ?
O6 Cl2 O6 108.1(4) 2_665 . ?
O6 Cl2 O6 108.1(4) 2_665 3_565 ?
O6 Cl2 O6 108.1(4) 3_565 . ?

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
Ni1 O1 C6 C5 30.6(4) . . . . ?
Ni1 O1 C6 C5 -82.6(4) 14_456 . . . ?
Ni1 O2 C12 C11 -179.6(3) 14_456 . . . ?
Ni1 O2 C12 C11 1.9(5) . . . . ?
Ni1 N1 C1 C2 -172.7(4) . . . . ?
Ni1 N1 C5 C4 174.5(4) . . . . ?
Ni1 N1 C5 C6 -4.8(5) . . . . ?
Ni1 N2 C7 C8 177.8(3) . . . . ?
Ni1 N2 C11 C10 -177.5(4) . . . . ?
Ni1 N2 C11 C12 2.5(5) . . . . ?
Ni2 O1 C6 C5 151.8(3) . . . . ?
N1 C1 C2 C3 -1.8(8) . . . . ?
N1 C5 C6 O1 -16.9(5) . . . . ?
N2 C7 C8 C9 -0.3(7) . . . . ?
N2 C11 C12 O2 -2.9(6) . . . . ?
C1 N1 C5 C4 -1.9(7) . . . . ?
C1 N1 C5 C6 178.8(4) . . . . ?
C1 C2 C3 C4 -0.5(9) . . . . ?
C2 C3 C4 C5 1.5(8) . . . . ?
C3 C4 C5 N1 -0.3(8) . . . . ?
C3 C4 C5 C6 179.0(5) . . . . ?
C4 C5 C6 O1 163.8(4) . . . . ?
C5 N1 C1 C2 3.0(7) . . . . ?
C7 N2 C11 C10 0.9(6) . . . . ?
C7 N2 C11 C12 -179.0(4) . . . . ?
C7 C8 C9 C10 0.5(8) . . . . ?
C8 C9 C10 C11 -0.1(8) . . . . ?
C9 C10 C11 N2 -0.7(7) . . . . ?
C9 C10 C11 C12 179.2(5) . . . . ?
C10 C11 C12 O2 177.2(4) . . . . ?
C11 N2 C7 C8 -0.4(6) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_date_sample_data_collection 2016-11-11
_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 '754o SOB'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 2.062
_oxdiff_exptl_absorpt_empirical_full_min 0.626
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 0 3 3.496

_platon_squeeze_details          
'approx 27 molecules of MeOH per unit cell masked with SQUEEZE'
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 0.167 475 138 ' '
2 0.000 0.000 0.500 473 138 ' '
3 -0.333 0.333 0.833 476 138 ' '

_platon_squeeze_void_probe_radius 1.20
_vrf_CHEMW03_3                   
;
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_2
_database_code_depnum_ccdc_archive 'CCDC 1819132'
_audit_update_record             
;
2018-01-24 deposited with the CCDC.
2018-03-15 downloaded from the CCDC.
;
# local name eb16225
_audit_creation_date             2016-09-23
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C72 H72 Cr2 N12 O12 Zn5, 5.91(Cl0.68 O2.71), 9 C H4 O'
_chemical_formula_sum            'C81 H108 Cl4 Cr2 N12 O37 Zn5'
_chemical_formula_weight         2414.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N10 O10 Zn Cl Cr'
_chemical_oxdiff_usercomment     '@ 120 K 713o'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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                   14.5920(3)
_cell_length_b                   14.5920(3)
_cell_length_c                   37.7623(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6963.4(4)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    12927
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.4140
_cell_measurement_theta_min      3.3900
_shelx_estimated_absorpt_T_max   0.848
_shelx_estimated_absorpt_T_min   0.610
_exptl_absorpt_coefficient_mu    1.706
_exptl_absorpt_correction_T_max  0.9900
_exptl_absorpt_correction_T_min  0.8357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0701 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.8441.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3720
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 2 -9 0.0700
0 -17 -19 0.0758
17 -18 -10 0.0896
18 0 10 0.1012
-3 18 19 0.1001
1 -1 -53 0.0088
-1 -1 53 0.0239
-17 18 10 0.0882

_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
-17.9999 2.0000 -8.9997 -0.0814 0.9161 0.3204
-0.0000 -16.9999 -18.9987 -0.0027 0.1207 1.0112
16.9999 -17.9999 -9.9990 0.0656 -0.7510 0.6591
17.9999 0.0000 9.9996 0.0600 -0.9308 -0.4311
-3.0000 17.9999 18.9986 0.0026 0.0275 -1.0025
1.0000 -1.0000 -52.9956 -0.9182 -0.0664 0.3833
-1.0000 -1.0000 52.9956 0.9572 0.0815 -0.2792
-16.9999 17.9999 9.9990 -0.0656 0.7510 -0.6591

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       -43
_diffrn_reflns_number            35087
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.792
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  33.00   1.00   20.00    --   -7.39 -99.00-120.00   53
  2  ω    -20.00  33.00   1.00   20.00    --   -7.39 -99.00 -30.00   53
  3  ω    -80.00  15.00   1.00   20.00    --   -7.39 -38.00-120.00   95
  4  ω    -20.00  49.00   1.00   20.00    --    8.80 -99.00  30.00   69
  5  ω    -64.00  -1.00   1.00   20.00    --    8.80 -38.00   0.00   63
  6  ω     -1.00  48.00   1.00   20.00    --    8.80 -99.00  90.00   49
  7  ω    -14.00  77.00   1.00   20.00    --    8.80  38.00 -60.00   91
  8  ω    -36.00  -9.00   1.00   20.00    --    8.80 -77.00  90.00   27
  9  ω     -6.00  79.00   1.00   20.00    --    8.80  19.00-150.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0064305000
_diffrn_orient_matrix_UB_12      -0.0194777000
_diffrn_orient_matrix_UB_13      0.0175729000
_diffrn_orient_matrix_UB_21      -0.0519410000
_diffrn_orient_matrix_UB_22      -0.0075657000
_diffrn_orient_matrix_UB_23      0.0004157000
_diffrn_orient_matrix_UB_31      -0.0202680000
_diffrn_orient_matrix_UB_32      -0.0520727000
_diffrn_orient_matrix_UB_33      -0.0066330000
_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                2599
_reflns_number_total             2846
_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         1.903
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2846
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0660
_refine_ls_restrained_S_all      1.149
_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)+(0.0247P)²+127.7921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1438
_refine_special_details          
;
One of the metal sites (Zn/Cr1) was modelled with subsitutional disorder and the ratio fixed such that the total formula of the wheel is Cr2Zn5.  The SQUEEZE routine of PLATON was used to handle 9 molecules of disordered methanol per complete wheel, which could not be modelled with discrete atoms.  This missing solvent is included in the total chemical formula, which triggers several checkCIF alerts that should be ignored.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.21 Report
341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0101 Ang.
906_ALERT_3_C Large K value in the Analysis of Variance ......      5.777 Check
906_ALERT_3_C Large K value in the Analysis of Variance ......      2.138 Check

Noted, but not significant

#===============================================================================
002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          9 Note
003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         11 Report

Noted, but not significant

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 ..     0.2059 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     127.79 Why ?

Consequence of disorder and SQUEEZE.  Discussed above.

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          4 Report
244_ALERT_4_G Low    'Solvent' Ueq as Compared to Neighbors of        Cl2 Check
300_ALERT_4_G Atom Site Occupancy of >Zn1    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 =         50 Note
304_ALERT_4_G Non-Integer Number of Atoms (   3.38) in Resd. #          2 Check
304_ALERT_4_G Non-Integer Number of Atoms (   1.62) in Resd. #          4 Check
432_ALERT_2_G Short Inter X...Y Contact  O4A    ..  C2      ..       3.01 Ang.
432_ALERT_2_G Short Inter X...Y Contact  O4A    ..  C2      ..       3.01 Ang.
432_ALERT_2_G Short Inter X...Y Contact  O4A    ..  C2      ..       3.01 Ang.
605_ALERT_4_G Largest Solvent Accessible VOID in Structure ...        466 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 .............         45 Note
869_ALERT_4_G ALERTS Related to the use of SQUEEZE Suppressed           ! Info
910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           4 Note
913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note

None of the above are serious problems.  Most pertain to the disorder in the model, or to the use of SQUEEZE, both of which 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
{Cr1, Zn1}
3. Restrained distances
 Cl1-O4 \\sim Cl1-O3 \\sim Cl1A-O3A \\sim Cl1A-O4A \\sim Cl2-O5 \\sim Cl2-O6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Cr1) = Uanis(Zn1)
5. Rigid body (RIGU) restrains
 Cl1A, O3A, O4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, O5, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C12
 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(Cl1A)=Sof(O4A)=0.33333*(1-FVAR(2))
 Sof(Cl1)=Sof(O4)=0.33333*FVAR(2)
 Sof(O3)=FVAR(1)
 Fixed Sof: Zn1(0.66666) 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
Zn1 Zn 0.57745(5) 0.73127(5) 0.17051(2) 0.0247(2) Uani 0.6667 1 d . . . A 2
Zn2 Zn 0.3333 0.6667 0.1667 0.0168(3) Uani 1 6 d S T P A .
Cr1 Cr 0.57745(5) 0.73127(5) 0.17051(2) 0.0247(2) Uani 0.3333 1 d . . . A 1
O1 O 0.4721(3) 0.7702(3) 0.19442(9) 0.0240(8) Uani 1 1 d . . . . .
O2 O 0.5247(2) 0.5883(3) 0.18953(10) 0.0256(8) Uani 1 1 d . U . . .
N1 N 0.6606(3) 0.8062(3) 0.21537(13) 0.0280(10) Uani 1 1 d . . . . .
N2 N 0.4050(3) 0.3833(3) 0.19776(12) 0.0254(10) Uani 1 1 d . . . . .
C1 C 0.7615(5) 0.8383(4) 0.22180(18) 0.0381(14) Uani 1 1 d . . . . .
H1 H 0.8029 0.8316 0.2037 0.046 Uiso 1 1 calc R . . . .
C2 C 0.8089(5) 0.8816(5) 0.2541(2) 0.0509(18) Uani 1 1 d . . . . .
H2 H 0.8813 0.9037 0.2581 0.061 Uiso 1 1 calc R . . . .
C3 C 0.7488(6) 0.8917(6) 0.2802(2) 0.0525(18) Uani 1 1 d . . . . .
H3 H 0.7792 0.9198 0.3026 0.063 Uiso 1 1 calc R . . . .
C4 C 0.6440(5) 0.8610(5) 0.27363(17) 0.0427(15) Uani 1 1 d . . . . .
H4 H 0.6018 0.8685 0.2913 0.051 Uiso 1 1 calc R . . . .
C5 C 0.6020(4) 0.8190(4) 0.24071(15) 0.0289(12) Uani 1 1 d . . . . .
C6 C 0.4880(4) 0.7823(4) 0.23167(14) 0.0280(12) Uani 1 1 d . . . . .
H6A H 0.4414 0.7140 0.2435 0.034 Uiso 1 1 calc R . . . .
H6B H 0.4691 0.8347 0.2404 0.034 Uiso 1 1 calc R . . . .
C7 C 0.3363(5) 0.2794(4) 0.20028(17) 0.0371(14) Uani 1 1 d . . . . .
H7 H 0.2802 0.2473 0.1836 0.045 Uiso 1 1 calc R . . . .
C8 C 0.3443(6) 0.2181(5) 0.2262(2) 0.0484(18) Uani 1 1 d . . . . .
H8 H 0.2934 0.1449 0.2279 0.058 Uiso 1 1 calc R . . . .
C9 C 0.4267(7) 0.2637(6) 0.2498(2) 0.059(2) Uani 1 1 d . . . . .
H9 H 0.4341 0.2220 0.2676 0.071 Uiso 1 1 calc R . . . .
C10 C 0.4986(6) 0.3700(5) 0.24753(19) 0.0486(17) Uani 1 1 d . . . . .
H10 H 0.5562 0.4031 0.2636 0.058 Uiso 1 1 calc R . . . .
C11 C 0.4845(5) 0.4278(4) 0.22094(16) 0.0326(13) Uani 1 1 d . . . . .
C12 C 0.5600(4) 0.5459(4) 0.21683(16) 0.0327(13) Uani 1 1 d . U . . .
H12A H 0.5644 0.5821 0.2395 0.039 Uiso 1 1 calc R . . . .
H12B H 0.6316 0.5587 0.2110 0.039 Uiso 1 1 calc R . . . .
Cl1 Cl 0.6667 0.3333 0.1742(2) 0.0342(18) Uani 0.677(19) 3 d DS TU P B 1
Cl1A Cl 0.6667 0.3333 0.1638(5) 0.042(5) Uani 0.323(19) 3 d DS TU P B 2
O3 O 0.6989(12) 0.4372(7) 0.1617(3) 0.049(3) Uani 0.677(19) 1 d D U . B 1
O3A O 0.695(3) 0.4364(15) 0.1762(7) 0.059(7) Uani 0.323(19) 1 d D U . B 2
O4 O 0.6667 0.3333 0.2122(3) 0.082(5) Uani 0.677(19) 3 d DS TU P B 1
O4A O 0.6667 0.3333 0.1261(6) 0.095(11) Uani 0.323(19) 3 d DS TU P B 2
Cl2 Cl 1.0000 1.0000 0.34511(7) 0.0544(8) Uani 1 3 d DS TU P . .
O5 O 1.0000 1.0000 0.3078(2) 0.064(2) Uani 1 3 d DS TU P . .
O6 O 0.9717(7) 0.8980(5) 0.35825(18) 0.107(3) Uani 1 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
Zn1 O1 2.092(3) . ?
Zn1 O1 2.183(4) 14_455 ?
Zn1 O2 1.971(3) 15 ?
Zn1 O2 1.964(3) . ?
Zn1 N1 2.052(5) . ?
Zn1 N2 2.051(4) 15 ?
Zn2 O1 2.102(3) . ?
Zn2 O1 2.102(3) 3_565 ?
Zn2 O1 2.102(3) 2_665 ?
Zn2 O1 2.102(3) 14_455 ?
Zn2 O1 2.102(3) 13_565 ?
Zn2 O1 2.102(3) 15 ?
Cr1 O1 2.183(4) 14_455 ?
Cr1 O1 2.092(3) . ?
Cr1 O2 1.964(3) . ?
Cr1 O2 1.971(3) 15 ?
Cr1 N1 2.052(5) . ?
Cr1 N2 2.051(4) 15 ?
O1 Zn1 2.183(4) 15 ?
O1 Cr1 2.183(4) 15 ?
O1 C6 1.423(6) . ?
O2 Zn1 1.971(3) 14_455 ?
O2 Cr1 1.971(3) 14_455 ?
O2 C12 1.424(6) . ?
N1 C1 1.325(7) . ?
N1 C5 1.356(7) . ?
N2 Zn1 2.051(4) 14_455 ?
N2 Cr1 2.051(4) 14_455 ?
N2 C7 1.338(7) . ?
N2 C11 1.334(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.389(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.373(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(8) . ?
C5 C6 1.510(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C7 C8 1.371(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.372(11) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.391(8) . ?
C11 C12 1.519(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Cl1 O3 1.424(8) 3_665 ?
Cl1 O3 1.424(8) 2_655 ?
Cl1 O3 1.424(8) . ?
Cl1 O4 1.434(12) . ?
Cl1A O3A 1.423(14) . ?
Cl1A O3A 1.423(14) 3_665 ?
Cl1A O3A 1.423(14) 2_655 ?
Cl1A O4A 1.422(15) . ?
Cl2 O5 1.408(8) . ?
Cl2 O6 1.421(6) 3_675 ?
Cl2 O6 1.421(6) . ?
Cl2 O6 1.421(6) 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 Zn1 O1 81.01(18) . 14_455 ?
O2 Zn1 O1 91.18(14) 15 14_455 ?
O2 Zn1 O1 100.36(14) . . ?
O2 Zn1 O1 77.67(14) 15 . ?
O2 Zn1 O1 75.68(14) . 14_455 ?
O2 Zn1 O2 166.85(14) . 15 ?
O2 Zn1 N1 94.43(16) . . ?
O2 Zn1 N1 97.95(16) 15 . ?
O2 Zn1 N2 81.30(16) 15 15 ?
O2 Zn1 N2 99.73(16) . 15 ?
N1 Zn1 O1 156.17(16) . 14_455 ?
N1 Zn1 O1 79.53(16) . . ?
N2 Zn1 O1 97.88(15) 15 14_455 ?
N2 Zn1 O1 158.91(16) 15 . ?
N2 Zn1 N1 105.22(18) 15 . ?
O1 Zn2 O1 180.0 2_665 14_455 ?
O1 Zn2 O1 82.68(12) . 14_455 ?
O1 Zn2 O1 97.32(12) 13_565 14_455 ?
O1 Zn2 O1 82.68(12) 3_565 14_455 ?
O1 Zn2 O1 180.0 3_565 15 ?
O1 Zn2 O1 97.32(12) 15 14_455 ?
O1 Zn2 O1 82.68(12) 2_665 15 ?
O1 Zn2 O1 97.32(12) 2_665 . ?
O1 Zn2 O1 82.68(12) . 15 ?
O1 Zn2 O1 180.0 . 13_565 ?
O1 Zn2 O1 82.68(12) 2_665 13_565 ?
O1 Zn2 O1 97.32(12) 2_665 3_565 ?
O1 Zn2 O1 97.32(12) . 3_565 ?
O1 Zn2 O1 97.32(12) 15 13_565 ?
O1 Zn2 O1 82.68(12) 3_565 13_565 ?
O1 Cr1 O1 81.01(18) . 14_455 ?
O2 Cr1 O1 77.67(14) 15 . ?
O2 Cr1 O1 75.68(14) . 14_455 ?
O2 Cr1 O1 100.36(14) . . ?
O2 Cr1 O1 91.18(14) 15 14_455 ?
O2 Cr1 O2 166.85(14) . 15 ?
O2 Cr1 N1 97.95(16) 15 . ?
O2 Cr1 N1 94.43(16) . . ?
O2 Cr1 N2 99.73(16) . 15 ?
O2 Cr1 N2 81.30(16) 15 15 ?
N1 Cr1 O1 79.53(16) . . ?
N1 Cr1 O1 156.17(16) . 14_455 ?
N2 Cr1 O1 158.91(16) 15 . ?
N2 Cr1 O1 97.88(15) 15 14_455 ?
N2 Cr1 N1 105.22(18) 15 . ?
Zn1 O1 Zn1 97.31(13) . 15 ?
Zn1 O1 Zn2 99.45(14) . . ?
Zn2 O1 Zn1 96.61(14) . 15 ?
Zn2 O1 Cr1 96.61(14) . 15 ?
Cr1 O1 Zn2 99.45(14) . . ?
Cr1 O1 Cr1 97.31(13) . 15 ?
C6 O1 Zn1 111.3(3) . . ?
C6 O1 Zn1 118.2(3) . 15 ?
C6 O1 Zn2 128.4(3) . . ?
C6 O1 Cr1 111.3(3) . . ?
C6 O1 Cr1 118.2(3) . 15 ?
Zn1 O2 Zn1 109.31(17) . 14_455 ?
Cr1 O2 Cr1 109.31(17) . 14_455 ?
C12 O2 Zn1 133.7(3) . . ?
C12 O2 Zn1 116.9(3) . 14_455 ?
C12 O2 Cr1 116.9(3) . 14_455 ?
C12 O2 Cr1 133.7(3) . . ?
C1 N1 Zn1 126.6(4) . . ?
C1 N1 Cr1 126.6(4) . . ?
C1 N1 C5 119.1(5) . . ?
C5 N1 Zn1 114.2(3) . . ?
C5 N1 Cr1 114.2(3) . . ?
C7 N2 Zn1 126.6(4) . 14_455 ?
C7 N2 Cr1 126.6(4) . 14_455 ?
C11 N2 Zn1 114.5(3) . 14_455 ?
C11 N2 Cr1 114.5(3) . 14_455 ?
C11 N2 C7 118.8(5) . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.3(6) . . ?
C2 C1 H1 118.9 . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.6(6) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 119.9(6) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.8 . . ?
C3 C4 C5 118.4(6) . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 121.6(5) . . ?
N1 C5 C6 116.8(5) . . ?
C4 C5 C6 121.6(5) . . ?
O1 C6 C5 110.5(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 119.0 . . ?
N2 C7 C8 122.0(6) . . ?
C8 C7 H7 119.0 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.2(6) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.8(6) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 121.0 . . ?
C9 C10 C11 118.0(7) . . ?
C11 C10 H10 121.0 . . ?
N2 C11 C10 122.3(6) . . ?
N2 C11 C12 116.5(5) . . ?
C10 C11 C12 121.2(6) . . ?
O2 C12 C11 110.6(4) . . ?
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 . . ?
O3 Cl1 O3 109.6(8) 2_655 . ?
O3 Cl1 O3 109.6(8) 3_665 2_655 ?
O3 Cl1 O3 109.6(8) 3_665 . ?
O3 Cl1 O4 109.4(8) 3_665 . ?
O3 Cl1 O4 109.4(8) 2_655 . ?
O3 Cl1 O4 109.4(8) . . ?
O3A Cl1A O3A 109.7(15) . 2_655 ?
O3A Cl1A O3A 109.7(15) 3_665 2_655 ?
O3A Cl1A O3A 109.7(15) 3_665 . ?
O4A Cl1A O3A 109.2(15) . 2_655 ?
O4A Cl1A O3A 109.2(15) . . ?
O4A Cl1A O3A 109.2(15) . 3_665 ?
O5 Cl2 O6 110.4(3) . 3_675 ?
O5 Cl2 O6 110.4(3) . . ?
O5 Cl2 O6 110.4(3) . 2_765 ?
O6 Cl2 O6 108.5(3) 2_765 3_675 ?
O6 Cl2 O6 108.5(3) . 3_675 ?
O6 Cl2 O6 108.5(3) . 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
Zn1 O1 C6 C5 29.0(5) . . . . ?
Zn1 O1 C6 C5 -82.4(5) 15 . . . ?
Zn1 O2 C12 C11 178.0(3) . . . . ?
Zn1 O2 C12 C11 -3.7(6) 14_455 . . . ?
Zn1 N1 C1 C2 -175.2(5) . . . . ?
Zn1 N1 C5 C4 175.2(4) . . . . ?
Zn1 N1 C5 C6 -3.1(6) . . . . ?
Zn1 N2 C7 C8 -175.5(4) 14_455 . . . ?
Zn1 N2 C11 C10 177.1(5) 14_455 . . . ?
Zn1 N2 C11 C12 -3.0(6) 14_455 . . . ?
Zn2 O1 C6 C5 151.3(3) . . . . ?
Cr1 O1 C6 C5 -82.4(5) 15 . . . ?
Cr1 O1 C6 C5 29.0(5) . . . . ?
Cr1 O2 C12 C11 178.0(3) . . . . ?
Cr1 O2 C12 C11 -3.7(6) 14_455 . . . ?
Cr1 N1 C1 C2 -175.2(5) . . . . ?
Cr1 N1 C5 C4 175.2(4) . . . . ?
Cr1 N1 C5 C6 -3.1(6) . . . . ?
Cr1 N2 C7 C8 -175.5(4) 14_455 . . . ?
Cr1 N2 C11 C10 177.1(5) 14_455 . . . ?
Cr1 N2 C11 C12 -3.0(6) 14_455 . . . ?
N1 C1 C2 C3 -0.4(10) . . . . ?
N1 C5 C6 O1 -17.6(6) . . . . ?
N2 C7 C8 C9 -1.7(10) . . . . ?
N2 C11 C12 O2 4.4(7) . . . . ?
C1 N1 C5 C4 -2.5(8) . . . . ?
C1 N1 C5 C6 179.1(5) . . . . ?
C1 C2 C3 C4 -1.3(11) . . . . ?
C2 C3 C4 C5 0.9(10) . . . . ?
C3 C4 C5 N1 1.0(9) . . . . ?
C3 C4 C5 C6 179.2(6) . . . . ?
C4 C5 C6 O1 164.1(5) . . . . ?
C5 N1 C1 C2 2.2(8) . . . . ?
C7 N2 C11 C10 0.2(8) . . . . ?
C7 N2 C11 C12 -179.9(5) . . . . ?
C7 C8 C9 C10 1.2(11) . . . . ?
C8 C9 C10 C11 -0.1(11) . . . . ?
C9 C10 C11 N2 -0.7(10) . . . . ?
C9 C10 C11 C12 179.5(6) . . . . ?
C10 C11 C12 O2 -175.8(5) . . . . ?
C11 N2 C7 C8 1.0(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-09-20
_olex2_date_sample_submission    2016-09-20
_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 713o
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.886
